Method for producing a sulphided copper sorbent

Patent metadata

Field	Value
Publication number	US-9873617-B2
Application number	US-201314382171-A
Country	US
Kind code	B2
Filing date	Feb 25, 2013
Priority date	Mar 16, 2012
Publication date	Jan 23, 2018
Grant date	Jan 23, 2018

Abstract

A method for producing a sulphided copper sorbent includes the steps of: (i) contacting a sorbent precursor material containing one or more sulphidable copper compounds, with a sulphiding gas stream including hydrogen sulphide to form a sulphided sulphur-containing sorbent material, and (ii) subjecting the sulphided sulphur-containing sorbent material to a heating step in which it is heated to a temperature above that used in the sulphiding step and ≧110° C., under an inert gas selected from nitrogen, argon, helium, carbon dioxide, methane, and mixtures thereof, the inert gas optionally including hydrogen sulphide. The method provides sulphided copper sorbents that have reduced levels of elemental sulphur.

First claim

The invention claimed is:

1. A method for producing a sulphided copper sorbent, comprising the steps of: (i) contacting a sorbent precursor material containing one or more sulphidable copper compounds, with a sulphiding gas stream comprising hydrogen sulphide and an inert gas selected from nitrogen, argon, helium, carbon dioxide, methane, and mixtures thereof to form a sulphided sulphur-containing sorbent material, and (ii) subjecting the sulphided sulphur-containing sorbent material to a heating step in which it is heated to a temperature above that used in the sulphiding step and ≧110° C., under a gas consisting of an inert gas selected from nitrogen, argon, helium, carbon dioxide, methane, and mixtures thereof, or a gas consisting of hydrogen sulphide and an inert gas selected from nitrogen, argon, helium, carbon dioxide, methane, and mixtures thereof.

2. A method according to claim 1 wherein the precursor is formed by combining an oxide, hydroxide, carbonate or hydroxycarbonate of copper or copper and zinc, with one or more binders or by combining an oxide, hydroxide, carbonate or hydroxycarbonate of copper or copper and zinc, with one or more binders and a support material.

3. A method according to claim 1 wherein the sorbent precursor is formed by impregnating a support material with a solution of a soluble salt of copper, followed by drying the impregnated support or by impregnating a support material with a solution of a soluble salt of copper, followed by drying and calcining the impregnated support.

4. A method according to claim 1 wherein the sorbent precursor is formed by coating a support material with a slurry of an insoluble copper compound, followed by drying the coated support or by coating a support material with a slurry of an insoluble copper compound, followed by drying and calcining the coated support.

5. A method according to claim 2 wherein the support material is selected from the group consisting of alumina, hydrated alumina, metal-aluminate, silica, titania, zirconia, zinc oxide, aluminosilicates, zeolites, or a mixture thereof.

6. A method according to claim 1 wherein the hydrogen sulphide content of the sulphiding gas stream is 0.25 to 80% by volume.

7. A method according to claim 1 where the pressure of the sulphiding gas stream is in the range 1 to 100 psig.

8. A method according to claim 1 wherein the sulphiding gas stream comprises an oxidant selected from one or more of free oxygen (O 2 ), sulphur oxides and nitrogen oxides, and has a total oxidant content of ≦1%.

9. A method according to claim 1 wherein the inlet temperature for the sulphiding step is in the range 0-150° C.

10. A method according to claim 1 wherein the sulphiding gas stream is passed through a fixed bed of the sorbent precursor at a linear velocity ≧0.1 m/s but less than the fluidization velocity.

11. A method according to claim 1 wherein the sulphiding gas stream comprises water vapour.

12. A method according to claim 1 wherein the sulphiding gas stream has a water vapour level in the range 0.2 to 2.0% by volume.

13. A method according to claim 1 wherein the sulphur-containing sorbent material is heated to a temperature in the heating step that is 40 or more degrees centigrade higher than the maximum temperature in the sulphiding step.

14. A method according to claim 1 wherein the sulphur-containing sorbent material is heated to a temperature ≧125° C.

15. A method according to claim 1 wherein the sorbent precursor comprises basic copper carbonate and the sulphur-containing sorbent material is heated to a temperature in the range 140 to 200° C.

16. A method according to claim 1 wherein the heating step is performed under an inert gas selected from nitrogen, argon, helium, carbon dioxide, methane, and mixtures thereof, said inert gas comprising hydrogen sulphide at a concentration lower than that used in the sulphiding step.

17. A method according to claim 1 further comprising reducing the sulphided sorbent material in a hydrogen containing gas stream to produce a reduced copper sorbent.

18. A method according to claim 1 wherein the hydrogen sulphide content of the sulphiding gas stream is 0.5 to 10% by volume.

19. A method according to claim 1 wherein the hydrogen sulphide content of the sulphiding gas stream is 0.75 to 4.5% by volume.

20. A method according to claim 1 where the pressure of the sulphiding gas stream is in the range 1 to 20 psig.

21. A method according to claim 1 wherein the sulphiding gas stream comprises an oxidant selected from one or more of free oxygen (O 2 ), sulphur oxides and nitrogen oxides, and has a total oxidant content of ≦0.01% by volume.

22. A method according to claim 1 wherein the inlet temperature for the sulphiding step is in the range 20-100° C.

23. A method according to claim 1 wherein the sulphur-containing sorbent material is heated to a temperature ≧140° C.

24. A method according to claim 1 wherein the sorbent precursor comprises basic copper carbonate and the sulphur-containing sorbent material is heated to a temperature in the range 160 to 200° C.

25. A method according to claim 1 wherein the sorbent precursor comprises basic copper carbonate and the sulphur-containing sorbent material is heated to a temperature in the range 160 to 180° C.

Assignees

• Cousins Matthew John
• Davis David
• Rafferty Paul
• Ridley Sarah
• Tapster Alan Gordon
• Johnson Matthey Plc

Inventors

• Cousins Matthew John
• Davis David
• Rafferty Paul
• Ridley Sarah
• Tapster Alan Gordon

Classifications

• B01J20/3236

  containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts · CPC title

• B01D2256/24

  Hydrocarbons · CPC title

• C10L3/101

  Removal of contaminants · CPC title

• C10G29/10

  Sulfides · CPC title

• B01J20/2803

  Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products · CPC title