Method for applying a wash coat suspension to a carrier structure

• US 8,722,565 B2
• Filed: 06/02/2008
• Issued: 05/13/2014
• Est. Priority Date: 05/31/2007
• Status: Active Grant

• Current Assignee: Clariant Produkte Deutschland GmbH (Clariant AG)
• Original Assignee: Sued-Chemie IP GmbH & Co., KG (Clariant AG)
• Inventors: Mestl, Gerhard, Estenfelder, Marvin, Gckel, Christian, Kding, Bastian
• Primary Examiner(s): Mayes, Melvin C
• Assistant Examiner(s): NGUYEN, COLETTE B
• Application Number:
  US12/601,876
• Publication Number:
  US 20100311573A1
• Time in Patent Office: 2,171 Days
• Field of Search: None
• US Class Current: 502/170
• CPC Class Codes: B01J 2/16 by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain
• CPC Class Codes: B01J 23/002 Mixed oxides other than spinels, e.g. perovskite
• CPC Class Codes: B01J 23/22 Vanadium
• CPC Class Codes: B01J 23/881 and iron
• CPC Class Codes: B01J 23/8885 containing also molybdenum
• CPC Class Codes: B01J 2523/00 Constitutive chemical elements of heterogeneous catalysts
• CPC Class Codes: B01J 2523/15 Caesium
• CPC Class Codes: B01J 2523/17 Copper
• CPC Class Codes: B01J 2523/47 Titanium
• CPC Class Codes: B01J 2523/51 Phosphorus
• CPC Class Codes: B01J 2523/53 Antimony
• CPC Class Codes: B01J 2523/55 Vanadium
• CPC Class Codes: B01J 2523/68 Molybdenum
• CPC Class Codes: B01J 2523/69 Tungsten
• CPC Class Codes: B01J 35/40 characterised by dimensions, e.g. grain size in a colloidal state B01J35/23; crystallite size B01J35/77
• CPC Class Codes: B01J 37/0232 by pulverisation
• CPC Class Codes: C07C 57/04 Acrylic acid; Methacrylic acid

Abstract

A method for applying a washcoat suspension to a support structure. To provide coatings with largely uniform thickness starting from washcoat suspensions, the method uses a device (10) set up to produce, by means of a process gas (40), a fluid bed of support structures in which the support structures circulate elliptically or toroidally, the method comprising the steps of:

• a) charging the device (10) with support structures and producing a support-structure fluid bed by means of a process gas (40), wherein the support structures circulate in the fluid bed elliptically or toroidally, preferably toroidally;
• b) impregnating the support structures with a washcoat suspension by spraying the support structures circulating elliptically or toroidally in the fluid bed with the washcoat suspension;
• c) drying the support structures sprayed with the washcoat suspension; and
• d) optionally calcining the support structures loaded with the solids contents of the washcoat suspension.

Claims

1. A method for applying a washcoat suspension to a support structure, wherein the method is carried out using a device (10) which is set up to produce, by means of a process gas (40) a fluid bed of support structures in which the support structures circulate elliptically or toroidally said method comprising the steps of:

a) charging the device (10) with support structures and producing a support-structure fluid bed by means of a process gas (40), wherein the support structures circulate in the fluid bed elliptically or toroidally;

b) impregnating the support structures with a washcoat suspension by spraying the support structures circulating elliptically or toroidally in the fluid bed with the washcoat suspension;

c) drying the support structures sprayed with the washcoat suspension; and

d) optionally calcining the support structures loaded with the solids contents of the washcoat suspension.

2. The method according to claim 1, wherein the device (10) comprises a process chamber (15) with a bottom (16) in the centre of which bottom an annular gap nozzle (50) is arranged.

3. The method according to claim 2, wherein the process chamber (15) furthermore comprises a side wall (18), wherein the process gas (40) is fed, with a horizontal movement component aligned radially outwards, into the process chamber (15) through the bottom (16) of the process chamber (15), the bottom being constructed of several overlapping annular guide plates laid one over the other (25, 26, 27, 29) between which annular slots (28) are formed, in order to produce the support-structure fluid bed.

4. The method according to claim 3, wherein the process gas (40) fed into the process chamber (15) is subjected to a circumferential flow component.

5. The method according to claim 4, wherein the process gas (40) fed into the process chamber (15) is subjected to the circumferential flow component by means of guide elements which are arranged between the annular guide plates (25, 26, 27, 29).

6. The method according to claim 4, wherein the process gas (40) fed into the process chamber (15) is subjected to the circumferential flow component by feeding an additional process gas (61), with a movement component aligned diagonally upwards, through the bottom (16) of the process chamber (15) into the process chamber (15) in the area of the side wall (18) of the process chamber (15).

7. The method according to claim 2, wherein the annular gap nozzle (50) atomizes a spray cloud (70) of the washcoat suspension which runs parallel to the plane of the bottom (16).

8. The method according to claim 7, wherein the mouth (55) of the annular gap nozzle (50) is embedded into the fluid bed.

9. The method according to claim 7, wherein a gas support cushion (72) is produced on the underside of the spray cloud (70).

10. The method according to claim 1, wherein the support structure is formed from a non-porous material or material mixture comprising steatite, quartz (SiO₂), porcelain, magnesium oxide, tin dioxide, silicon carbide, rutile, alumina (Al₂O₃), aluminium silicate, magnesium silicate, zirconium silicate, cerium silicate or mixtures of two or more of the above materials.

11. The method according to claim 1, wherein the support structure has a hardness greater than/equal to 20 N.

12. The method according to claim 1, wherein the process gas (40) is selected from the group consisting of air, oxygen, nitrogen and the noble gases.

13. The method according to claim 1, wherein the process gas (40) is heated, preferably to a temperature of more than/equal to 40°

C.

14. The method according to claim 1, wherein the process gas (40) is enriched, before being fed into the process chamber (15), with the suspending agent of the washcoat suspension in a range of 10 to 50% of the saturation vapour pressure.

15. The method according to claim 1, wherein the support structure is formed as a sphere, cylinder, perforated cylinder, trilobe, tetralobe, ring, doughnut, star, cartwheel or strand.

16. The method according to claim 1, wherein the washcoat suspension contains TiO₂, V₂O₅ and Sb₂O₃ in particulate form.

17. The method according to claim 16, wherein the suspension furthermore comprises a phosphate compound, an alkali and/or alkaline earth compound, and an organic and/or inorganic binding agent.

18. The method according to claim 16, wherein the washcoat suspension is sprayed onto a ring as support structure.

19. The method according to claim 1, wherein the washcoat suspension contains iron molybdate.

20. The method according to claim 1, wherein the washcoat suspension contains a mixed oxide of Mo, V and W, or Mo, V and Nb, or Ta as well as optionally Te or Sb, which is optionally doped with Cu, Mn or Fe.

21. The method of claim 1, wherein a device (10) produces, by means of a process gas (40), a fluid bed of support structures in which the support structures circulate elliptically or toroidally for applying a washcoat suspension to a support structure.

22. The method of claim 21, wherein the device (10) comprises a process chamber (15) with a bottom (16) in the centre of which bottom an annular gap nozzle (50) is arranged.

23. The method of claim 22, wherein the process chamber (15) furthermore comprises a side wall (18), wherein the bottom (16) is constructed of several overlapping annular guide plates laid one over another (25, 26, 27, 29) between which annular slots (28) are formed via which process gas (40) can be fed in with a horizontal movement component aligned radially outwards.

24. The method of claim 23, wherein guide elements which impose a circumferential flow component on the process gas passing through are arranged between the annular guide plates (25, 26, 27, 29).

25. The method of claim 22, wherein the mouth (55) of the annular gap nozzle (50) is formed such that with the nozzle (50) a spray cloud (70) can be sprayed which runs parallel to the bottom plane.

26. The method of claim 25, wherein outlets (59) for support gas are provided between the mouth (55) of the annular gap nozzle (50) and the bottom (16) lying beneath it, in order to produce a support cushion on the underside of the spray cloud (70).

27. The method of claim 26, wherein the support gas can be provided by the annular gap nozzle (50) itself and/or by the process gas (40).

28. The method of claim 22, wherein the annular gap nozzle (50) has a conical head (57), and in that the mouth (55) runs along a circular circumferential line of a conical section.

29. The method of claim 22, wherein there is arranged in the area between the mouth (55) of the nozzle (50) and the bottom (16) lying beneath it a truncated-cone-shaped or hyperbolic wall (58) which preferably has passage openings (59) for support gas.

30. The method of claim 29, wherein an annular slot (60) for the passage of process gas (40) is formed between the underside of the truncated-cone-shaped or hyperbolic wall (58) and the bottom (16) lying beneath it.

31. The method of claim 22, wherein the position of the mouth (55) of the nozzle (50) is height-adjustable.

32. A shell catalyst produced according to the method of claim 1, comprising a shaped body to which a shell comprising a metal-oxide material is applied, wherein the shell catalyst is an element of a batch of a plurality of shell catalysts, wherein the ratio of the standard deviation of the shell thicknesses of the shell catalysts of the batch to the mean value of the shell thicknesses of the shell catalysts of the batch is smaller than/equal to 20%.