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1. (WO2019028127) SORBANTS À BASE D'OXYDE DE ZINC UTILISANT DES HYDROXYDES DE MÉTAUX ALCALINS ET LEURS PROCÉDÉS DE PRÉPARATION ET D'UTILISATION
Note: Texte fondé sur des processus automatiques de reconnaissance optique de caractères. Seule la version PDF a une valeur juridique

CLAIMS

What is claimed is:

1. A fluidizable, attrition-resistant sorbent for removing at least one reduced sulfur species from a feed stream comprising:

substantially spherical particles, said particles comprising at least 75 wt% of an active zinc component consisting essentially of a zinc oxide phase and a zinc aluminate phase, each of said phases having a crystallite size of less than about 50 nm as determined by x-ray diffraction line broadening analysis,

said active zinc component having a total zinc oxide content, calculated based on the combined zinc oxide of said zinc oxide phase and said zinc aluminate phase, of from about 50 wt%, to about 80 wt%, based on the weight of said active zinc component, wherein the residual sodium level in the solid phase is in the range of between 25 parts per million by weight of sodium and 2500 parts per million by weight of sodium.

2. The fluidizable, attrition-resistant sorbent of claim 1, wherein the residual sodium level in the solid phase is in the range of between 50 parts per million by weight of sodium and 1000 parts per million by weight of sodium.

3. The fluidizable, attrition-resistant sorbent of claim 1, wherein the residual sodium level in the solid phase is in the range of between 75 parts per million by weight of sodium and 750 parts per million by weight of sodium.

4. The fluidizable, attrition-resistant sorbent of any of claims 1-3, wherein the reduced sulfur species is ¾S.

5. A fluidizable, attrition-resistant sorbent for removing COS from a feed stream comprising: substantially spherical particles, said particles comprising at least 75 wt% of an active zinc component consisting essentially of a zinc oxide phase and a zinc aluminate phase, each of said phases having a crystallite size of less than about 50 nm as determined by x-ray diffraction line broadening analysis,

said active zinc component having a total zinc oxide content, calculated based on the combined zinc oxide of said zinc oxide phase and said zinc aluminate phase, of from about 50 wt%, to about 80 wt%, based on the weight of said active zinc component, wherein the residual sodium level in the solid phase is in the range of between 25 parts per million by weight of sodium and 2500 parts per million by weight of sodium.

6. A process for preparing a fluidizable, attrition resistant, active zinc oxide containing sorbent comprising the steps:

forming a first slurry by combining an aqueous solution of a zinc oxide precursor and aluminum oxide precursor with an aqueous solution of an alkali metal hydroxide such that the solids content comprises a precipitated zinc oxide precursor and a precipitated aluminum oxide precursor, said precipitated zinc oxide precursor and said precipitated aluminum oxide precursor being present in an amount, calculated as ZnO, and AI2O3, respectively, such that said precipitated zinc oxide precursor constitutes between about 50 wt%, and about 80 wt%, of the total solids content of said precipitated zinc oxide precursor and said precipitated aluminum oxide precursor in said slurry, and such that the pH of this slurry during the mixing and combining step is maintained between the values of 5.5 and 7.5;

separating the liquid phase of the first slurry from the solid phase by a separating means; washing the filtered solid phase with water, preferably deionized water, to achieve a residual sodium level in the solid phase of between 25 parts per million by weight of sodium and 2500 parts per million by weight of sodium;

treating the separated solid material from the first slurry with water and concentrated acid to generate a second slurry wherein the pH of the second slurry is adjusted with acid to be between 3.5 and 5.0;

spray drying the second slurry to form spray dried particles; and

calcining said spray dried particles to provide fluidizable, attrition resistant, active zinc oxide containing sorbent particles comprising a two-phase component consisting essentially of a zinc oxide phase and a zinc aluminate phase.

7. The process of claim 6, wherein said spray drying step is conducted under conditions sufficient to provide calcined particles having a size range of between 35 μιη and 175 μιη.

8. The process of any of claims 6-7, wherein said zinc oxide constitutes at least about 50 wt% of the total solids content of said zinc oxide precursor and said aluminum oxide precursor in said slurry.

9. The process of any of claims 6-8, wherein the active zinc oxide containing sorbent particles comprise zinc oxide grains less than 50 nm diameter.

10. The process of any of claims 6-8, wherein the active zinc oxide containing sorbent particles comprise zinc oxide grains about 10 nm to about 40 nm diameter.

11. The process of any of claims 6-8, wherein the active zinc oxide containing sorbent particles comprise zinc oxide grains about 12 nm to about 30 nm diameter.

12. The process of any of claims 6-8, wherein the active zinc oxide containing sorbent particles comprise zinc oxide grains about 13 nm to about 20 nm diameter.

13. The process of any of claims 6-12, wherein said slurry additionally comprises at least one additional material selected from the group consisting of promoter precursors, binder precursors and refractory oxide precursors, and wherein said additional material is present in amount selected to provide fluidizable, attrition resistant, active zinc oxide containing sorbent particles containing at least about 75 wt% of said two-phase component consisting essentially of a zinc oxide phase and a zinc aluminate phase.

14. The process of claim 13, wherein said additional material is present in amount selected to provide fluidizable, attrition resistant, active zinc oxide containing sorbent particles containing at least about 80 wt% of said two-phase component consisting essentially of a zinc oxide phase and a zinc aluminate phase.

15. The process of claim 14, wherein said additional material is present in amount selected to provide fluidizable, attrition resistant, active zinc oxide containing sorbent particles containing at least about 90 wt% of said two-phase components consisting essentially of a zinc oxide phase and a zinc aluminate phase.

16. The process of claim 15, wherein said additional material is present in amount selected to provide fluidizable, attrition resistant, active zinc oxide containing sorbent particles containing at least about 95 wt% of said two-phase component consisting essentially of a zinc oxide phase and a zinc aluminate phase.

17. The process of any of claims 6-16, wherein all or part of the alkali metal hydroxide is replaced with an alkali metal carbonate.

18. The process of any of claims 6-16, wherein the alkali metal hydroxide is sodium hydroxide.

19. The process of claim 18, wherein all or part of the sodium hydroxide is replaced with sodium carbonate.

20. The process of any of claims 6-19, wherein the residual sodium level in the solid phase is between 50 parts per million by weight of sodium and 1000 parts per million by weight of sodium.

21. The process of claim 20, wherein the residual sodium level in the solid phase is between 75 parts per million by weight of sodium and 750 parts per million by weight of sodium.

22. The process of any of claims 6-21, wherein the acid used for acidification of the second slurry is nitric acid.

23. The process of any of claims 6-22, wherein the pH range of the second slurry is adjusted to be between 4.0 and 4.5.

24. The process of any of claims 6-23, wherein the formation of the first slurry is performed at a temperature of ambient to about 85 °C.

25. The process of claim 24, wherein the formation of the first slurry is performed at a temperature of about 50°C to about 80°C.

26. The process of claim 25, wherein the formation of the first slurry is performed at a temperature of about 65 °C to about 75 °C.

27. The process of any of claims 6-26, wherein the separating of the liquid phase of the first slurry from the solid phase includes a washing process performed at temperatures between ambient and about 85°C.

28. The process of any of claims 6-27, wherein the separating of the liquid phase of the first slurry from the solid phase includes a washing process performed at temperatures between about 50°C and about 80°C.

29. The process of any of claims 6-28, wherein said spray dried particles are calcined at about 500°C to about 900°C.

30. The process of claim 29, wherein said spray dried particles are calcined at about 600°C to about 800°C.