CA2017980A1 - Distillation column reactor - Google Patents

Distillation column reactor

Info

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
Application number
CA002017980A
Other languages
French (fr)
Inventor
Edward M. Jones, Jr.
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chemical Research and Licensing Co
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of CA2017980A1 publication Critical patent/CA2017980A1/en
Abandoned legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/16Fractionating columns in which vapour bubbles through liquid
    • B01D3/18Fractionating columns in which vapour bubbles through liquid with horizontal bubble plates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20Chemical 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
    • B01J8/22Chemical 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
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S203/00Distillation: processes, separatory
    • Y10S203/06Reactor-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.

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.
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.

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.
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.
CA002017980A 1989-06-07 1990-05-31 Distillation column reactor Abandoned CA2017980A1 (en)

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)

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WO2016020374A1 (en) * 2014-08-05 2016-02-11 Basf Se Column for the thermal treatment of a fluid, having a return line

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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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