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Catalytic Distillation Structure Europa,schesP_ MM M II M M MM M M Ml M M I II J European Patent Office © Publication number: 0 458 472 B1 Office europeen des brevets^ © EUROPEAN PATENT SPECIFICATION © Date of publication of patent specification: 15.03.95 © Int. CI.6: B01 D 3/00, B01J 8/02, B01J 35/04 © Application number: 91303834.5 @ Date of filing: 26.04.91 © Catalytic distillation structure. ® Priority: 21.05.90 US 526444 Qj) Proprietor: CHEMICAL RESEARCH & LICENS- ING COMPANY @ Date of publication of application: 10100 Bay Area Boulevard 27.11.91 Bulletin 91/48 Pasadena, Texas 77507 (US) © Publication of the grant of the patent: 15.03.95 Bulletin 95/11 @ Inventor: Adams, John R. 15223 Park Estates Lane © Designated Contracting States: Houston, BE DE ES FR GB IT NL SE Texas 77062 (US) © References cited: GB-A- 2 096 603 © Representative: Cropp, John Anthony David et US-A- 4 302 356 al US-A- 4 443 559 MATHYS & SQUIRE US-A- 4 536 373 100 Grays Inn Road London, WC1X 8AL (GB) 00 CM 00 Note: Within nine months from the publication of the mention of the grant of the European patent, any person ® may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition CL shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee LU has been paid (Art. 99(1) European patent convention). Rank Xerox (UK) Business Services (3. 10/3.09/3.3.3) 1 EP 0 458 472 B1 2 Description trays in a distillation column reactor. So far, the most commercially successful ar- BACKGROUND OF THE INVENTION rangement has been to the place the particulate catalyst in closed pockets disposed along a fiber Field of the Invention 5 glass cloth belt. The main problems sought to be overcome by The present invention relates to structures the improvements have been the reduction of pres- which can be used in reactions wherein the reac- sure drop through the column and provision of tion and distillation of the reaction mixture are sufficient contact of the reactants with the catalyst carried on concurrently using the structures as both io while providing for good vapor liquid contact for the catalyst for the reaction and as distillation struc- fractional distillation. Many useful catalysts are in tures. More particularly the present invention re- the form of fine particulate powders which preclude lates to a rigid container having distillation surfaces their use directly as distillation components. Even thereon, the container being filled with a particulate larger extruded pellets do not lend themselves well catalyst component. 75 as distillation structures. Hence the use of cloth belts, cages and support trays. While larger cata- Related Art lysts structures have been proposed, the porosity requirements of many catalytic materials limit their A new method of carrying out catalytic reac- structural integrity. Many catalysts which rely on tions has been developed, wherein the components 20 outer surface activity only and which might have of the reaction mixture are concurrently separable the strength for larger structures are useful only for by fractional distillation. Several systems have gas phase reactions, such as maleic anhydride been proposed and one commercially successful production. uses the catalyst as the catalytic distillation struc- ture. Such a system is variously described in U.S. 25 SUMMARY OF THE INVENTION patents 4,215,011; 4,232,177; 4,242,530; 4,250,052; 4,302,356; 4,307,254; 4,336,407; 4,439,350; The present invention provides catalytic distilla- 4,443,559; and 4,482,775. tion structures which are useful in the concurrent Briefly, the commercial structure described reaction and distillation of a reaction mixture. The therein comprises a cloth belt with a plurality of 30 distillation structures are provided as small rigid pockets spaced along the belt and containing par- containers. The catalyst component is loaded into ticulate catalyst material. The cloth belt with cata- the containers and the containers closed off. Al- lyst filled pockets is wound into a helix about a though the containers are closed off, openings are spacing material such as knitted stainless steel provided to allow vapor and liquid passage into and wire mesh, and these "bales" loaded into a distilla- 35 out of the containers. A multitude of catalyst con- tion column. Additionally U.S. patents 4,443,559 tainers are placed into a distillation column which and 4,250,052 disclose a variety of catalyst struc- then becomes a reactor/distillation column. The tures for this use. surfaces of the containers provide the necessary Placing the particulate catalyst loose on stan- vapor/liquid contact surfaces for the distillation. The dard distillation trays has also been proposed. See, 40 rigidity of the containers provides for spacing the for example, U.S. Pat. No. 4,215,011 and U.K. structures and the necessary free space for the patents GB 2,096,603 and 2,096,604. The place- distillation. ment of the catalyst in the downcomers of standard In particular, the present invention relates to a distillation columns has been proposed as in U.S. catalytic distillation structure for use as packing patent 3,634,534. Fluidization of the catalyst on the 45 material in a distillation column reactor, comprising trays has also been suggested as in U.S. patent a particulate catalyst component disposed in a rigid 4,471,154. Some deficiencies of such fluidized container having openings thereon to allow free beds were recognized in Chemiker passage of liquid and vapours, the container sur- Zeitung/Chemische Apparatur, vol. 90, no. 13, July faces providing the distillation contact surfaces, 1966 and U.S. Pat. No. 4,215,011. Quang, et al, in 50 said container being substantially smaller in volume U.S. Pat. No. 4,847,430 and Nocca, et al in U.S. than said distillation column reactor volume. Pat. No. 4,847,431 disclose loading the particulate In one embodiment of this invention, the rigid catalyst on alternating trays of a distillation column container of the catalytic distillation structure re- and with a gas by pass about the catalyst loaded ferred to above comprises a hollow cylinder closed trays. 55 at both ends and having openings in the ends and An alternative arrangement is described in US- wall to allow liquid and vapour to enter and leave A-4 536 373 where the catalyst is housed in porous said container, both the length and diameter of the containers which are supported on the distillation hollow cylinder are substantially smaller than the 2 3 EP 0 458 472 B1 4 corresponding dimensions of the distillation column lytic distillation structure container of reactor. FIG. 2 having radially extending fins In a second embodiment of this invention, the along one side of each of the slotted rigid container comprises a hollow cylinder having openings. an inner wall extending generally parallel to the 5 FIG. 4 is a depiction of a cylindrical catalytic cylindrical wall of the cylinder and having the ends distillation structure container having closed to divide the space within the cylinder into a circular openings in the ends and lon- hollow central space which is open at both ends gitudinally spiralled slotted openings and a second space surrounding the central space in the wall. which is closed at both ends. The catalyst compo- io FIG. 5 is a depiction of an annular cylindrical nent is disposed in the second closed space. This catalytic distillation structure container second space has openings in the ends and walls wherein the catalyst component is which allow liquid and vapour to enter and leave disposed within the inner cylindrical the space. Both the length and diameter of the space. container are substantially smaller than the cor- is FIG. 6 is a depiction of an annular cylindrical responding dimensions of the distillation column catalytic distillation structure container reactor. wherein the catalyst component is In a third embodiment of the present invention, disposed within the annular space. the rigid container comprises a hollow cylinder which is closed at both ends and which has an 20 DESCRIPTION OF THE PREFERRED EMBODI- inner wall extending generally parallel to the cylin- MENTS drical wall of the cylinder dividing the space within the cylinder into a closed central space and a The present invention provides catalytic struc- second closed space surrounding said central tures which can be used as distillation structures. space, said catalyst component being disposed in 25 In order to serve both functions there are three said central space and said ends and walls having highly desirable criteria. First, the structure should openings to allow liquid and vapour to pass through be such as to provide for relatively even spatial said second space and pass into and out of said dispersion in the distillation column reactor. That is, central space. the catalyst structures rest in the column in a In each of these embodiments, the openings 30 geometric arrangement which will perform the de- may comprise circular ports in the ends and wall or sired functions of reaction and distillation sites. To walls of the rigid container. In one alternative ar- achieve this these structures may be such as to rangement, the openings may comprise circular provide fairly uniform spatial distribution in the col- ports in the ends and longitudinally slotted ports in umn. the wall or walls of the rigid container. In one 35 A second criteria is that there be sufficient free preferred arrangement, a longitudinal fin extends space in the catalyst bed to allow for the liquid radially from one side of each of said slotted ports.
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