Process for preparing a spent catalyst for precious metals recovery

Patent metadata

Field	Value
Publication number	US-9580770-B2
Application number	US-201414521195-A
Country	US
Kind code	B2
Filing date	Oct 22, 2014
Priority date	Oct 22, 2014
Publication date	Feb 28, 2017
Grant date	Feb 28, 2017

Abstract

A process is provided for preparing a spent noble metal fixed-bed catalyst for precious metals recovery, comprising: a) adding the catalyst to a caustic solution to wash the spent catalyst and to make a wash slurry having an alkaline pH, wherein the spent catalyst has been in contact with chloroaluminate ionic liquid catalyst, and wherein the spent catalyst comprises from 5 to 35 wt % chloride; and b) filtering the wash slurry and collecting: i) a filter cake having from at least 70 wt % of the chloride in the spent catalyst removed and having the noble metals retained, and ii) a wash filtrate. Also provided is a filter cake comprising a washed consolidated cake having 40 to 75 wt % solids, a cake moisture content from 25 to less than 60 wt %, 0.1 to 1.5 wt % total noble metals, and a residual chloride content of from zero to less than 4 wt %.

First claim

It is claimed:

1. A process comprising:
a. adding a spent noble metal fixed-bed catalyst comprising one or more noble metals to a caustic solution to wash the spent noble metal fixed-bed catalyst and to make a wash slurry having a pH from 7 to 12.5, wherein the spent catalyst has been in contact with a chloroaluminate ionic liquid catalyst, and wherein the spent catalyst comprises from 5 to 35 wt % chloride; and
b. filtering the wash slurry and collecting: i) a filter cake having from at least 70 wt % to 100 wt % of the chloride in the spent catalyst removed and having from 90 wt % to 100 wt % of the one or more noble metals retained, and ii) a wash filtrate.

2. The process of claim 1 , wherein the spent noble metal fixed-bed catalyst comprises one or more platinum group metals.

3. The process of claim 1 , wherein the pH of the wash slurry is from 9 to 12.

4. The process of claim 1 , wherein the spent noble metal fixed-bed catalyst has been used for hydro-regeneration of the chloroaluminate ionic liquid catalyst.

5. The process of claim 1 , additionally comprising adding a filter aid to the wash slurry.

6. The process of claim 5 , wherein the filter aid comprises from 70 to 99 wt % silica.

7. The process of claim 5 , wherein an amount of the filter aid added to the wash slurry is from 10,000 to 30,000 ppmw, on a total solids basis.

8. The process of claim 5 , wherein filtering of the wash slurry is at a filter wash flux rate of 3.0 to 12.0 Lpm/m 2 .

9. The process of claim 1 , wherein the filter cake has a washed filter cake thickness from greater than 5 to 25 mm.

10. The process of claim 1 , wherein the filter cake has a cake moisture content from 25 to 60 wt %.

11. The process of claim 1 , wherein an amount of water used to wash the filter cake is from 0.20 to 1.00 gallons of water per pound of the spent catalyst.

12. The process of claim 1 , wherein the wash filtrate has a wash filtrate pH from 9.0 to 12.0.

13. The process of claim 1 , wherein the spent catalyst is pelleted and has a pellet diameter from 1.0 to 10.0 mm.

14. The process of claim 1 , wherein exotherms of up to 40° C. above ambient temperature occur during the adding of the spent catalyst to the caustic solution.

15. The process of claim 1 , wherein the filtering uses a filter medium with a pore size from 1 to 100 microns.

16. The process of claim 1 , wherein the caustic solution comprises from 40 to 150 grams of sodium hydroxide per liter of water.

17. The process of claim 1 , wherein a time between the adding and the filtering of the wash slurry is from 10 to 60 minutes.

18. The process of claim 1 , wherein the filter cake comprises from 0 to less than 4 wt % residual chloride.

19. The process of claim 1 , additionally comprising rinsing of the filter cake with a water rinse, and wherein a total amount of water used to wash and rinse the filter cake is less than 1.00 gallons per pound of the spent catalyst.

20. The process of claim 1 , wherein:
an amount of a filter aid greater than 15,000 ppmw, on a total solids basis, is added to the wash slurry,
the filtering of the wash slurry is at a filter wash flux rate of greater than 3.5 to 12 Lpm/m 2 ,
the filter cake has a washed filter cake thickness from greater than 5 to 25 mm,
the filter cake has a cake moisture content from 25 to less than 60 wt %, and
greater than 70% of the chloride in the spent catalyst is removed, prior to any subsequent rinsing of the filter cake.

21. The process of claim 1 , additionally comprising recovering the one or more noble metals using a metallurgical extraction technique comprising re-pulping, grinding, and leaching the filter cake in a hot alkaline cyanide solution to provide dissolved platinum group metals, liquid-solid separation of the dissolved platinum group metals, and recovering the dissolved platinum group metals using a strong base anion exchange resin or by cementation with cementation metals comprising aluminum or zinc.

Assignees

• Bhaduri Rahul Shankar
• Timken Hye Kyung Cho
• Cuspard Philip Ian
• Chevron Usa Inc

Inventors

• Bhaduri Rahul Shankar
• Timken Hye Kyung Cho
• Cuspard Philip Ian

Classifications

• B01J2219/00177

  controlling the pH · CPC title

• B01J38/64 Primary

  using alkaline material; using salts · CPC title

• C22B7/009

  General processes for recovering metals or metallic compounds from spent catalysts (for recovering specific metals C22B11/00 - C22B61/00) · CPC title

• C22B11/048 Primary

  from spent catalysts · CPC title

• B01J23/96

  of catalysts comprising metals, oxides or hydroxides of the noble metals · CPC title