Alumina particles

• US 4,952,389 A
• Filed: 09/15/1989
• Issued: 08/28/1990
• Est. Priority Date: 09/15/1989
• Status: Expired due to Term

• Current Assignee: Norton Company (Compagnie De Saint-Gobain)
• Original Assignee: Norton Company (Compagnie De Saint-Gobain)
• Inventors: Szymanski, Thomas, Remus, Donald J., Butcher, Kenneth R.
• Primary Examiner(s): ROSENBERG, PETER
• Application Number:
  US07/407,845
• Time in Patent Office: 347 Days
• Field of Search: 423/625, 501/127, 501/118
• US Class Current: 423/625
• CPC Class Codes: B01J 21/04 Alumina
• CPC Class Codes: B01J 35/30 characterised by their physical properties
• CPC Class Codes: B01J 35/31 Density
• 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 35/60 characterised by their surface properties or porosity
• CPC Class Codes: B01J 35/612 less than 10 m2/g
• CPC Class Codes: C01F 7/025 Granulation or agglomeration
• CPC Class Codes: C01P 2004/32 Spheres
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2006/11 Powder tap density
• CPC Class Codes: C01P 2006/12 Surface area
• CPC Class Codes: C01P 2006/21 Attrition-index or crushing strength of granulates

Abstract

Essentially spherical particles are disclosed of at least 98.5% alumina having a surface area less than about 1 m² /g, an attrition resistance of less than about 0.3 weight percent/hour in an air jet attrition test, a particle size of about 30 to about 110 microns, a tap density of about 1.3 to about 1.9 g/cc, and sufficient porosity to hold catalytic metals in conventional catalytic amounts. The alumina particles are especially suited for use as fluid bed catalyst carriers for use in environments involving the presence of steam, particularly at high temperatures.

Claims

1. Friable particles having an alumina content of at least about 98.5 weight percent, a surface area of less than about 1 m² /g, an attrition resistance of less than about 0.3 weight % per hour when tested in an air jet apparatus, a particle size ranging from about 30 to about 110 microns, a tap density of about 1.3 to about 1.9 g/cc, a generally spherical shape, and sufficient porosity to hold catalytic quantities of catalytic metals.

2. The particles of claim 1, wherein they contain about 1.0 weight percent or less of silica and about 0.1 weight percent or less each of iron and alkali metals.

3. The particles of claim 1, wherein the surface area is less than about 0.3 m² /g.

4. The particles of claim 1, wherein the particles have an attrition resistance of less than about 0.2 weight %/hr.

5. The particles of claim 1, wherein the particles have an attrition resistance of less than about 0.15 weight %/hr.

6. The particles of claim 1 having an average particle size of about 40 to about 70 microns.

7. The particles of claim 1, wherein the tap density is less than about 1.8 g/cc.

8. The particles of claim 1, wherein the tap density is less than about 1.75 g/cc.

9. The particles of claim 1, wherein they have sufficient porosity to hold catalytic metals without increasing the amount of attrited material in an air jet attrition test by more than about 30 percent as compared to non-metal coated particles.

10. The particles of claim 1, wherein they have sufficient porosity to hold catalytic metals without increasing the amount of attrited material in an air jet attrition test by more than about 20 percent as compared to non-metal coated particles.

11. A process for preparing friable particles having an alumina content of at least about 98.5 weight percent, a surface area of less than about 1 m² /g, an attrition resistance of less than about 0.3 weight percent per hour when tested in an air jet apparatus, a particle size ranging from about 30 to about 110 microns, a tap density of about 1.3 to about 1.9 g/cc, a generally spherical shape, and sufficient porosity to hold catalytic quantities of catalytic metals, said process comprising the steps of (i) forming an aqueous slurry having about 15 to about 50 weight percent solids wherein the solids comprise about 85 to about 99 weight percent -325 U.S. mesh of a high fired alumina having an ultimate crystallite size of greater than about 25 microns, and about 1 to about 15 weight percent of a material selected from the group consisting of (a) a super ground alpha alumina having a particle size less than about 5 microns, (b) a clay, and (c) a mixture of (a) and (b);

(ii) spray drying the slurry to produce substantially spherical particles having an average particle size of about 30 to about 110 micron;

(iii) heat treating the spray dried particles at a temperature below their melting points to form agglomerates of alumina particles having a surface area below about 1 m² /g and an attrition resistance of less than about 0.3 weight %/hour in an air jet apparatus; and

(iv) deagglomerating the agglomerates to produce the particles.

12. The process of claim 11, wherein the high fired alumina is a tabular alumina

13. The process of claim 11, wherein the alpha alumina has a particle size of less than about 3 microns.

14. The process of claim 11, wherein the clay is a montmorillonite.

15. The process of claim 14, wherein the clay is bentonite and it is used in an amount up to about 2 weight percent of the solids of the aqueous slurry.

16. The process of claim 11, wherein the spray dried particles have an average particle size of about 40 to about 70 microns.

17. The process of claim 11, wherein the heat treating is performed at a temperature of up to about 1540°

C.

18. The process of claim 11, wherein the aqueous slurry further contains a dispersant.

19. The process of claim 18, wherein the dispersant is an ammonium polymethacrylate.

20. The process of claim 11, wherein the spray drying is performed at a temperature of about 100°

to about 350°

C.

21. A process for producing friable particles having an alumina content of at least about 99.5 weight percent, a surface area of less than about 1 m² /g, an attrition resistance of less than about 0.3 weight percent per hour when tested in an air jet apparatus, a particle size ranging from about 30 to about 110 microns, a tap density of about 1.3 to about 1.9 g/cc, a generally spherical shape, and sufficient porosity to hold catalytic quantities of catalytic metals, said process comprising (i) heating hydrated alumina particles having a particle size of about 35 to about 150 microns to remove at least about 90 weight percent of the bound water and to convert the hydrate to at least gamma alumina and (ii) entraining the particles in a carrier gas and passing them through a high temperature zone of a plasma spray at a temperature sufficient to at least partially melt the particles and to cause them to have the properties.

22. The process of claim 21, wherein the hydrated alumina is gibbsite.

23. The process of claim 21, wherein the heating is at a temperature of at least about 600°

C.

24. The process of claim 21, wherein the heating converts at least a portion of the hydrate to alpha alumina and the heating is at a temperature of at least about 1100°

C.

25. The process of claim 21, wherein the plasma spray is performed formed with a nitrogen torch gas at a torch gas flow of about 50 to 500 SCFH;

torch power of at least 10 KW;

nitrogen enthalpy of about 10,000 to about 30,000 BTU/lb; and

a particle feed rate of about 10 to about 75 lb/hr.

26. The process of claim 21, wherein the plasma spray is performed under the following conditions:

nitrogen torch gas;

torch gas flow of about 100 to 150 SCFH;

torch power of 60 KW;

nitrogen enthalpy of about 12,000 to about 16,000 BTU/lb; and

a particle feed rate of about 30 to about 50 lb/hr.