Process for catalyst unloading facilitation

Abstract

A process for facilitating the unloading of a fixed bed of cobalt/metal oxide catalyst particles from a reactor tube by (i) feeding a gas comprising 10 to 30 (vol/vol) percent of oxygen to the reactor tube with a GHSV for oxygen of 0.5 to 50 Nl/l/hr, and (ii) removing the catalyst particles from the reactor tube. In the fixed bed of catalyst particles to which the oxygen comprising gas is fed in step (i) at most 10 mole % of the element cobalt is present in Co3O4 and/or CoO, calculated on the total amount of moles of cobalt in the catalyst particles.

Claims

1. A process for facilitating the unloading of a fixed bed of catalyst particles from a reactor tube, the catalyst particles comprising: at least 40 weight % of a metal oxide chosen from the group of titania, silica, alumina, zirconia, ceria, gallia and mixtures thereof, and at least 2 weight % of the element cobalt, calculated on the total weight of the catalyst particles; the process comprising the steps of: (i) feeding a gas comprising 10 to 30 (vol/vol) percent of oxygen, to the reactor tube with a gas hourly space velocity for oxygen of 0.5 to 50 Nl/l/hr; and (ii) removing the catalyst particles from the reactor tube; wherein in the fixed bed of catalyst particles to which the oxygen comprising gas is fed in step (i) at most 10 mole % of the element cobalt is present in Co3O4 and/or CoO, calculated on the total amount of moles of cobalt in the catalyst particles.

2. The process as claimed in of claim 1, wherein in step (i) the oxygen comprising gas is air.

3. The process of claim 1, wherein the total pressure in the reactor tube during step (i) is in the range of 1 to 10 bar absolute.

4. The process of claim 1, wherein the gas hourly space velocity of oxygen is 1 to 20 Nl/l/hr.

5. The process of claim 1, wherein the fixed catalyst bed is subjected to washing with gas oil and/or subjected to a hydrogen containing gas before performing step (i).

6. The process of claim 1, wherein the reactor tube comprises steel, carbon steel and/or stainless steel.

7. The process of claim 1, wherein step (i) is performed while cooling the reactor tube from the outside, and wherein the temperature of the reactor tube at the cooling side is in the range of between 50 and 400 C.

8. The process of claim 1, wherein step (i) is performed while the oxygen comprising gas fed to the reactor has a temperature in the range of between 0 and 300 C.

9. The process of claim 1, wherein step (i) is performed in a once through operation.

10. The process of claim 1, wherein step (i) is performed by feeding the oxygen comprising gas from the top to the bottom of the reactor tube, or from the bottom to the top of the reactor tube.

11. The process of claim 1, wherein the catalyst particles comprise at least 40 weight % of titania, silica, alumina, zirconia or mixtures thereof, and at least 3 weight % of the element cobalt, calculated on the total weight of the catalyst particles, and optionally ruthenium.

12. The process according to claim 11, wherein the catalyst particles comprise at least 40 weight % and up to 97 weight % of titania, silica, alumina, zirconia or mixtures thereof, and at least 3 weight % up to 35 weight % of the element cobalt, calculated on the total weight of the catalyst particles, and optionally ruthenium.

13. The process of claim 11, wherein the catalyst particles have been prepared by means of co-extrusion of a metal oxide chosen from the group of titania, silica, alumina, zirconia, ceria, gallia and mixtures thereof and -cobalt and optionally ruthenium, followed by drying and/or calcination of the extrudates.

14. The process of claim 1, wherein the catalyst particles are Fischer Tropsch catalyst particles.

15. The process of claim 1, wherein in the fixed bed of catalyst particles to which the oxygen comprising gas is fed in step (i), at least 10 mole %, of the element cobalt is present as metallic cobalt and/or is present in cobalt carbide, calculated on the total amount of moles of cobalt in the catalyst particles.

Description

EXAMPLES

(1) Fixed beds of cobalt/titana catalysts were unloaded from several reactor tubes. For some the normal unloading method was used. For others the method of the present invention was used, whereby in step (ii) the normal unloading method was used.

(2) The catalyst particles in all fixed beds comprised more than 70 wt % of titania, and about 20 wt % of the element cobalt, calculated on the total weight of the catalyst particles.

(3) The catalyst particles had a size larger than 1 mm.

Procedure for Examples According to the Invention

(4) Before step (i) the catalyst comprised less than 0.1 mole % of the element cobalt in Co3O4 and/or CoO, and more than 30 mole % of the element cobalt present as metallic cobalt and present in cobalt carbide, calculated on the total amount of moles of cobalt in the catalyst particles.

(5) During step (i) a gas comprising 21% oxygen and having a temperature in the range of 20-30 C. was fed to the reactor with a GHSV of 6 Nl/l/hr. The cooling temperature of the water around the catalyst tubes was about 150 C. The total pressure in the reactor tube during step (i) was about 1.7 bar absolute.

(6) In step (ii) the normal unloading method was used to remove the catalyst particles from the reactor tube.

Results

(7) The fixed beds that were unloaded using a method according to the present invention were removed more quickly from the reactor tubes as compared to the fixed beds that were unloaded according to the normal unloading method. An improvement of 8 days was achieved.