Embodiments of the invention relate to processes and apparatus for the washing and recovery of metal-containing catalyst solids in a form suitable for reclamation. More specifically, a catalyst recovery process comprises removing an organic residue with a washing medium from a metal-containing catal
Embodiments of the invention relate to processes and apparatus for the washing and recovery of metal-containing catalyst solids in a form suitable for reclamation. More specifically, a catalyst recovery process comprises removing an organic residue with a washing medium from a metal-containing catalyst solids, recovering washed solids, and treating the washed solids under oxidative conditions to form non-reactive solids. The treatment oxidative conditions may be effective to convert the metal(s) into an oxide form and/or may facilitate the removal of remaining organic residue from the washed solids. The treatment of the washed solids may comprise calcination. In some embodiments, the metal-containing catalyst solids may be recovered from a slurry stream, and the process further comprises passing the slurry stream though a separation unit to obtain a catalyst-enriched retentate slurry. In some embodiments, the organic residue comprises a hydrocarbon wax, and the solid catalyst is a hydrocarbon synthesis particulate catalyst.
대표청구항▼
What is claimed is: 1. A process for recovering a solid metal-containing catalyst from a slurry, said process comprising: a) providing a catalyst slurry feedstream comprising a solid catalyst and wax hydrocarbons, said solid catalyst including a metallic component; b) optionally, adding a second fe
What is claimed is: 1. A process for recovering a solid metal-containing catalyst from a slurry, said process comprising: a) providing a catalyst slurry feedstream comprising a solid catalyst and wax hydrocarbons, said solid catalyst including a metallic component; b) optionally, adding a second feedstream to the catalyst slurry feedstream; c) passing the catalyst slurry feedstream through a solid-liquid separation unit to separate said slurry feedstream into a liquid stream and a retentate stream, both of which exit the solid-liquid separation unit, wherein the retentate stream is enriched in solid catalyst, and has a content in wax hydrocarbons that is less than the catalyst slurry feedstream; d) contacting the solid catalyst with a washing medium in a manner effective to displace some of the wax hydrocarbons and wash the solid catalyst; and e) treating the washed solid catalyst under conditions sufficient to convert the metallic component into a non-reactive form to generate non-reactive solids, wherein said conditions in step e) comprise exposing said washed solid catalyst to an oxidizing gas or oxidizing atmosphere comprising steam. 2. The process according to claim 1 wherein the solid-liquid separation unit comprises a rotary filtration unit. 3. The process according to claim 1 wherein either or both of the second feedstream and the washing medium composes an organic solvent. 4. The process according to claim 1 wherein step e) is carried out at a temperature that is greater than the highest of the boiling point and end boiling point temperature of the second feedstream and the washing medium. 5. The process according to claim 1 wherein the washing medium comprises steam. 6. The process according to claim 1 wherein at least one of steps b) through e) includes adding heat. 7. The process according to claim 1 wherein either or both of the second feedstream and the washing medium comprises a viscosity-reducing organic solvent. 8. The process according to claim 1 wherein either or both of the second feedstream and the washing medium comprises an organic solvent that dissolves at least some of the wax hydrocarbons from the solid catalyst structure. 9. The process according to claim 1 wherein the conditions in step e) comprise passing an oxidizing gas to contact the washed solid catalyst, wherein the oxidizing gas comprises steam and O2. 10. The process according to claim 1 wherein step e) is carried out at 450-600�� C. 11. The process according to claim 1, further comprising the following step: f) removing at least a portion of the remaining hydrocarbons from the washed solid catalyst using a stripping gas. 12. The process according to claim 1 wherein step a) comprises withdrawing a catalyst-containing slurry stream from a slurry bed reactor. 13. The process according to claim 1 wherein the solid catalyst comprises a metallic component selected from the group consisting of cobalt, ruthenium, and combinations thereof. 14. The process according to claim 1 wherein the metallic component of the catalyst comprises cobalt, and further comprises another element selected from the group consisting of silver, platinum, rhenium, boron, ruthenium, and combinations thereof. 15. The process according to claim 1 wherein step d) is carried out at the same time or in the same unit as step c). 16. An integrated process for producing hydrocarbons and recovering spent solid catalyst, comprising: a) contacting a hydrocarbon synthesis solid catalyst with a feedstream comprising carbon monoxide and hydrogen in a reaction zone under conversion promoting conditions to produce one or more hydrocarbons, wherein the hydrocarbon synthesis solid catalyst comprises a metal, and further wherein a deactivation of said solid catalyst takes place over time within said reaction zone to form spent solid catalyst; b) withdrawing at least a portion of the hydrocarbon synthesis solid catalyst from the reaction zone to provide a slurry feedstream comprising liquid hydrocarbons and solids, wherein the slurry solids comprising at least a portion of the spent solid catalyst; c) optionally, performing at least one step selected from the group consisting of: adjusting the hydrocarbon content of said slurry feedstream; adjusting the hydrocarbon composition of said slurry feedstream; adjusting the solids content of said slurry feedstream, and combinations thereof; d) separating the slurry feedstream into a liquid stream and a solids-enriched stream, wherein the liquid stream comprises most of the liquid hydrocarbons, and further wherein the solids-enriched stream comprises spent solid catalyst and remaining hydrocarbons; e) treating the solids-enriched stream under oxidative conditions sufficient to oxidize the catalyst metal to a non-zero oxidation state and optionally to remove the remaining hydrocarbons in order to generate oxidized metal-containing solids, wherein said treating step comprises exposing said solids-enriched stream to an oxidizing gas or oxidizing atmosphere comprising steam; and f) collecting the oxidized metal-containing solids for reclamation. 17. The process according to claim 16, wherein the collecting step comprises transporting the solids on a cooling conveyor. 18. The process according to claim 16 wherein step a) is carried out in a slurry bed reactor. 19. The process according to claim 16 wherein the solid catalyst comprises a metal selected from the group consisting of cobalt, ruthenium, and combinations thereof. 20. The process according to claim 16 wherein the conditions in said oxidative treatment step e) are such that said oxidized metal-containing solids are generated as a wet catalyst powder comprising a water content of up to 50 wt %. 21. The process according to claim 16 wherein said oxidizing gas or atmosphere in said oxidative treatment step (e) further comprises O2. 22. The process according to claim 16 wherein said oxidizing gas in said oxidative treatment step (e) further comprises a sulfur-containing compound. 23. The process according to claim 1 wherein said oxidizing gas in said oxidative treatment step (e) further comprises a sulfur-containing compound, and wherein said step e) provides a sulfided metal as a non-reactive form of said metallic component. 24. The process according to claim 1 wherein the conditions in said treatment step e) are such that said non-reactive solids are generated as a wet catalyst powder comprising a water content of up to 50 wt %. 25. A process for recovering a spent solid metal-containing catalyst from a slurry for reclamation, said process comprising: a) providing a catalyst slurry feedstream comprising a solid catalyst and wax hydrocarbons, said solid catalyst including a metallic component; b) optionally, adding a second feedstream to the catalyst slurry feedstream; c) passing the catalyst slurry feedstream through a solid-liquid separation unit to separate said slurry feedstream into a liquid stream and a retentate stream, both of which exit the solid-liquid separation unit, wherein the retentate stream is enriched in solid catalyst, and has a content in wax hydrocarbons that is less than the catalyst slurry feedstream; d) contacting the solid catalyst with a washing medium in a manner effective to displace some of the wax hydrocarbons and wash the solid catalyst, wherein step (d) is carried out in the separation unit of step (c); e) treating the washed solid catalyst under conditions sufficient to convert the metallic component into a non-reactive form to generate non-reactive solids; f) removing at least a portion of remaining hydrocarbons from the washed solid catalyst, said step (f) comprising stripping with a stripping gas, vaporizing by addition of heat, or combination thereof, wherein step (f) is carried out in the same unit as step (e); and g) collecting said non-reactive solids for reclamation.
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