Method for manufacturing a supported tantalum catalyst
A method for making a supported tantalum oxide catalyst precursor or catalyst with controlled Ta distribution and the resulting supported Ta catalyst. In an embodiment, the method comprises selecting a Ta-precursor with appropriate reactivity with the surface hydroxyls of the solid oxide support material to give a desired Ta distribution in the catalyst precursor or catalyst. In an embodiment the method comprises controlling the number of surface hydroxyls available on the support material to react with the Ta-precursor by thermal methods, such as calcination, to achieve the desired Ta distribution.
1. A method for making a supported tantalum oxide catalyst precursor with controlled Ta distribution, the method comprising:
providing a support comprising solid oxide or mixed oxide particles having a hydroxyl concentration;
selecting a Ta-precursor material having a reactivity that will provide a desired Ta distribution in the resulting tantalum oxide catalyst precursor particles;
contacting the solid oxide or mixed oxide particles with an organic solution containing the Ta-precursor material to form Ta-impregnated particles; and
recovering the Ta-impregnated particles to form a catalyst precursor comprising a desired Ta distribution,
wherein the method further comprises at least a chemical process to stabilize the Ta-precursor with at least one modifier in order to control the rate of reaction between the Ta-precursor and the support material.
2. The method of claim 1 , further comprising calcining the catalyst precursor to form a supported tantalum oxide catalyst comprising a desired Ta distribution.
3. The method of claim 1 , wherein the selected Ta-precursor material has a reaction rate with the solid oxide or mixed oxide particles that is faster than the mass transfer rate of the precursor towards the center of the particle.
4. The method of claim 3 , wherein the resulting catalyst precursor particles have an egg-shell distribution of Ta.
5. The method of claim 1 , wherein the selected Ta-precursor material has a reaction rate with solid oxide or mixed oxide particles that is approximate to or slower than the mass transfer rate of the precursor towards the center of the particle.
6. The method of claim 5 , wherein the resulting catalyst precursor particles have a uniform distribution of Ta throughout the particle.
7. The method of claim 1 , wherein the resulting catalyst precursor particles have a Ta:OH ratio that is below the OH-saturation level.
8. The method of claim 7 , wherein the Ta:OH ratio is less than 0.15.
9. The method of claim 1 , wherein the solid oxide or mixed oxide support comprises silica (SiO 2 ), alumina (Al 2 O 3 ), titania (TiO 2 ), zirconia (ZrO 2 ), hafnium oxide (HfO 2 ), magnesium oxide (MgO), silica-alumina, silica-zirconia, silica-titania, or combinations thereof.
10. The method of claim 9 , wherein solid oxide or mixed oxide particles have less than 5 wt % moisture.
11. The method of claim 9 , wherein the solid oxide or mixed oxide particles have an average diameter ranging from 0.5 to 5 mm.
12. The method of claim 9 , wherein the solid oxide or mixed oxide particles have an average surface area ranging from 200 to 600 m 2 /g.
13. The method of claim 9 , wherein the solid oxide or mixed oxide particles have an average pore volume ranging from 0.7 to 1.8 cc/g.
14. The method of claim 1 , wherein said contacting comprises adding the organic solution comprising the Ta-precursor material to the solid oxide or mixed oxide particles via incipient wetness impregnation or slurry reaction.
15. The method of claim 1 , wherein recovering the Ta-impregnated particles includes removing solvent that has been mixed with the Ta-precursor material.
16. The method of claim 1 , wherein said Ta-precursor comprises Ta-tetraethoxide-2,4-pentanedionate, Ta-ethoxide, or a combination of Ta-ethoxide and 2,4-pentanedione (acetyl acetone).
17. The method of claim 1 , wherein the Ta-precursor comprises Ta-ethoxide.
18. The method of claim 1 , wherein the modifier for the Ta-precursor comprises 2,4-pentanedione.
19. The method in claim 1 , wherein the Ta-precursor is Ta-ethoxide and the modifier is 2,4-pentanedione.
20. A method for making a supported tantalum oxide catalyst precursor with controlled Ta distribution, the method comprising:
providing a support comprising solid oxide or mixed oxide particles having hydroxyl groups attached thereto;
selecting a Ta-precursor material that has a desired reaction rate with said hydroxyl groups;
controlling the number of hydroxyl groups to react with said Ta-precursor by at least one thermal process;
contacting the solid oxide or mixed oxide particles having the controlled number of the hydroxyl groups with an organic solution comprising the Ta-precursor material to form Ta-impregnated particles; and
recovering the Ta-impregnated particles to form a catalyst precursor comprising a desired Ta distribution,
wherein the method further comprises at least a chemical process to stabilize the Ta-precursor with at least one modifier in order to control the rate of reaction between the Ta-precursor and the support material.
21. The method of claim 20 , further comprising calcining the catalyst precursor to form a supported tantalum oxide catalyst comprising a desired Ta distribution.
22. The method of claim 20 , wherein the thermal process comprises calcining the support to reduce the hydroxyl concentration thereon.