Supported metal oxides as catalysts for aldol condensations

• US 20050070733A1
• Filed: 12/02/2002
• Published: 03/31/2005
• Est. Priority Date: 12/06/2001
• Status: Active Grant

• Current Assignee: BASF AG (BASF SE)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Sigl, Marcus, Dobler, Walter, Miller, Christian, Haake, Mathias
• Granted Patent: US 7,098,366 B2
• Time in Patent Office: Days
• US Class Current: 560/210
• CPC Class Codes: B01D 3/009 in combination with chemical reactions
• CPC Class Codes: B01J 19/249 Plate-type reactors
• CPC Class Codes: B01J 19/32 Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
• CPC Class Codes: B01J 21/04 Alumina
• CPC Class Codes: B01J 2219/2453 Plates arranged in parallel
• CPC Class Codes: B01J 2219/2459 Corrugated plates
• CPC Class Codes: B01J 2219/2471 Feeding means for the catalyst
• CPC Class Codes: B01J 2219/2481 Catalysts in granular from between plates
• CPC Class Codes: B01J 2219/2497 Size aspects, i.e. concrete sizes are being mentioned in the classified document
• CPC Class Codes: B01J 2219/3221 Corrugated sheets
• CPC Class Codes: B01J 2219/32217 with sheets having corrugations which intersect at an angle of 90 degrees
• CPC Class Codes: B01J 2219/32227 Vertical orientation
• CPC Class Codes: B01J 2219/32237 Sheets comprising apertures or perforations
• CPC Class Codes: B01J 2219/32258 Details relating to the extremities of the sheets, such as a change in corrugation geometry or sawtooth edges
• CPC Class Codes: B01J 2219/32262 Dimensions or size aspects
• CPC Class Codes: B01J 2219/32408 Metal
• CPC Class Codes: B01J 2219/32466 comprising catalytically active material
• CPC Class Codes: B01J 2219/326 Mathematical modelling
• CPC Class Codes: B01J 23/10 of rare earths
• CPC Class Codes: B01J 23/92 of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
• CPC Class Codes: B01J 35/50 : characterised by their shape or configuration
• CPC Class Codes: B01J 8/003 : in a downward flow
• CPC Class Codes: B01J 8/0292 : with stationary packing material in the bed, e.g. bricks, wire rings, baffles
• CPC Class Codes: B01J 8/12 : moved by gravity in a downward flow
• CPC Class Codes: C07C 45/72 : by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
• CPC Class Codes: C07C 45/74 : combined with dehydration
• CPC Class Codes: C07C 49/203 : with only carbon-to-carbon double bonds as unsaturation
• CPC Class Codes: Y02P 20/10 : Process efficiency
• CPC Class Codes: Y02P 20/584 : Recycling of catalysts

Abstract

A supported catalyst is proposed comprising one or more metal oxides as active component on a catalyst support for carrying out an aldol condensation, with the catalyst support being γ-aluminum oxide, the active component comprising one or more oxides of the elements having atomic numbers 39 or from 57 to 71 and the concentration of the active component being in the range from 5 to 12% by weight, based on the weight of the catalyst support.

Claims

1-14. -14. (canceled)

15. A method of using supported catalyst consisting of one or more oxides of the elements having atomic numbers 39 or from 57 to 71 as active component on γ

-aluminum oxide as a catalyst support, the concentration of the active component being in the range from 5 to 12% by weight, based on the weight of the γ

-aluminum oxide catalyst support, for carrying out a heterogeneously catalyzed aldol condensation.

16. The method as claimed in claim 15, wherein the concentration of the active component is in the range from 7.5 to 10% by weight, based on the weight of the catalyst support.

17. The method as claimed in claim 15, wherein the geometry of the catalyst support is determined in such a manner that the ratio of the external surface area to the volume is in the range from 0.5 to 10 mm⁻

1.

18. The method as claimed in claim 15, wherein the active component is yttrium oxide.

19. The method as claimed in claim 15, wherein the active component is praseodymium oxide.

20. The method of using a column for carrying out an aldol condendsation by reactive distillation in the presence of a heterogeneous particulate catalyst having a structured packing or random packings which form interstices in the column interior, in which the quotient of the hydraulic diameter for the gas flow through the structured packing or the random packings and the equivalent diameter of the catalyst particles is in the range from 2 to 20 in such a manner that the catalyst particles are introduced into the interstices, distributed and discharged loose under the action of gravity, and the catalyst particles are formed from a supported catalyst according to the definition in claim 15.

21. The method as claimed in claim 20, wherein the structured packing is preferably a cross-channel packing.

22. The method as claimed in claim 20, wherein the structured packing or the random packings have horizontal surface portions.

23. The method as claimed in claim 22, wherein the structured packing is formed from structured sheet metal packings for vertical installation into the column having linear corrugations which subdivide the structured sheet metal packing into corrugated surfaces, wherein the angle of inclination of the corrugated surfaces to the horizontal is in the range from 90 to 450.

24. The method as claimed in claim 20, wherein the structured packing or the random packings have a reduced resistance to flow at their surface.

25. The method as claimed in claim 21, wherein the structured packing is formed from rippled or corrugated layers, and between two rippled or corrugated layers in each case one flat intermediate layer is disposed, with the flat intermediate layers not extending to the edge of the structured packing or having, in the edge zone of the structured packing, an increased gas permeability.

26. The method as claimed in claim 21, wherein the structured packing is formed from structured sheet metal packings for vertical installation in to the column having a linear corrugations which subdivide the structured sheet metal packings into corrugated surfaces and which have a width a measured from corrugated edge to corrugated edge and perforations, wherein a proportion X of at least 60% of the perforations has a distance b of at most 0.4 a to the lower corrugated surface.

27. A process for preparing pseudoionone by aldolizing citral and acetone by reactive distillation in a column according to the definition in claim 20, which comprises operating the column with respect to its gas and liquid loading in such a manner that a maximum of from 50 to 95% of the flooding limit loading is reached.

28. A process for carrying out a heterogeneously catalyzed aldol condensation by reactive distillation in a column according to the definition in claim 20, which comprises the supported catalyst being regenerated by treatment with an aqueous alkaline solution, when the original catalyst activity decreases.

29. The method as claimed in claim 17, wherein the geometry of the catalyst support is determined in such a manner that the ratio of the external surface area to the volume is in the range from 1 to 5 mm⁻

1.

30. A method as claimed in claim 17, wherein the catalyst support is in the form of solid or hollow cylinders, spheres and honeycombs, trilobes or toothed wheels.

31. A method as claimed in claim 20, wherein the quotient of the hydraulic diameter for the gas flow through the structured packing or of the random packings and the equivalent diameter of the catalyst particles is in the range from 2 to 20.

32. A method as claimed in claim 23, wherein the angle of inclination of the corrugated surfaces to the horizontal is 60°

.

33. A method as claimed in claim 24, wherein the reduced resistance to flow at the surface of the structured packing or of the random packings is due to perforations and/or roughness of the material of the structured packing or of the random packings or by constructing the structured packing as expanded metal.

34. A method as claimed in claim 25, wherein the flat intermediate layers have holes in the edge zone of the structured packing.