IP Library Granted Patent US 11,148,961
Granted Patent B2
US 11,148,961 · App. 16/490,344 · Granted Oct 19, 2021

Process for treatment of wastewater

Inventors: Christian Nowottny (Nidderau, DE); Birger Lehr (Nidderau, DE); Hartmut Janitz (Nidderau, DE); Zhenggang Yu (Nanjing, CN); Li Chen (Shanghai, CN)
Assignees: HERAEUS DEUTSCHLAND GMBH & CO. KG; HERAEUS PRECIOUS METAL TECHNOLOGY (CHINA) CO., LTD.; HERAEUS SITE OPERATIONS GMBH & CO. KG
C02F1/42C02F1/004C02F1/56C02F1/64C02F1/66C02F2001/425C02F2101/203C02F2103/16C02F2301/08
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Quick Facts
Patent No.
US 11,148,961
App. No.
16/490,344
Granted
Oct 19, 2021
Kind
B2
Abstract

A process for the treatment of acidic wastewater which comprises hydrochloric acid, nitric acid as an optional component, 0.1 to 30 wt.-% of one or more dissolved metals selected from the group consisting of aluminum and heavy metals other than precious metals, and 10 to 500 wt.-ppm of at least one dissolved precious metal, wherein the process comprises the successive steps (1) to (5): (1) adjusting the pH value of the wastewater to 6 to 8 to produce a first composition comprising a first precipitate and an aqueous phase having a pH value in the range of 6 to 8, (2) adjusting the pH value of the first composition to >8 to 11 to produce a second composition comprising the first precipitate, a second precipitate and an aqueous phase having a pH value in the range of >8 to 11, (3) separating the precipitates from the aqueous phase, (4) passing the aqueous phase through a sand filter to produce an aqueous filtrate, and (5) passing the aqueous filtrate through a regenerative cation exchanger comprising an acidic cation exchanger resin with chelating groups and a downstream non-regenerative cation scavenger comprising a scavenger resin with chelating sulfur containing groups to produce an aqueous salt solution with a total content of dissolved aluminum plus dissolved precious metals plus dissolved heavy metals other than precious metals of 0.1 to 10.0 wt.-ppm.

Claims (22)

1. A process for the treatment of acidic wastewater which comprises hydrochloric acid, 0.1 to 30 wt.-% of one or more dissolved metals selected from the group consisting of aluminum and heavy metals other than precious metals, and 10 to 500 wt.-ppm of at least one dissolved precious metal, wherein the process comprises the successive steps (1) to (5):

(1) adjusting the pH value of the wastewater to 6 to 8 to produce a first composition comprising a first precipitate and an aqueous phase having a pH value in the range of 6 to 8,

(2) adjusting the pH value of the first composition to >8 to 11 to produce a second composition comprising the first precipitate, a second precipitate and an aqueous phase having a pH value in the range of >8 to 11,

(3) separating the precipitates from the aqueous phase,

(4) passing the aqueous phase through a sand filter to produce an aqueous filtrate, and

(5) passing the aqueous filtrate through a regenerative cation exchanger comprising an acidic cation exchanger resin with chelating groups followed by a downstream non-regenerative cation scavenger comprising a scavenger resin with chelating sulfur containing groups to produce an aqueous salt solution with a total content of dissolved aluminum plus dissolved precious metals plus dissolved heavy metals other than precious metals of 0.1 to 10.0 wt.-ppm, wherein the aqueous salt solution comprises a salt content which comprises as essential components: 1 to 15 wt.-% of alkali chloride, 0 to 5 wt.-% of calcium chloride and 0 to 5 wt.-% of alkali nitrate, wherein the wt.-% are in each case based on the aqueous salt solution.

2. The process of claim 1 , wherein the acidic wastewater has a pH value in the range of 0 to <6.

3. The process of claim 1 , wherein the wastewater is a mixture or a combination of more than one different wastewaters.

4. The process of claim 1 , wherein the wastewater originates from a precious metal extraction process and/or from a precious metal recycling process.

5. The process of claim 1 , wherein the adjustment of the pH value of step (1) is performed by mixing the acidic wastewater with one or more basic alkali compounds.

6. The process of claim 1 , wherein the adjustment of the pH value of step (2) is performed by mixing the first composition with one or more basic alkali compounds.

7. The process of claim 1 , wherein the solid-liquid separation of step (3) is supported by adding a flocculent to the second composition.

8. The process of claim 7 , wherein the flocculent comprises polyacrylamide and/or one or more derivatives thereof.

9. The process of claim 1 , wherein the separation of step (3) is performed batchwise or as a continuous process.

10. The process of claim 1 , wherein the chelating groups of the acidic cation exchanger resin comprise chelating iminodiacetate groups.

11. The process of claim 1 , wherein the chelating sulfur containing groups of the scavenger resin comprise chelating thiourea groups.

12. The process of claim 1 , further comprising a step (6) of pH adjustment of the aqueous salt solution to a pH value in the range of 6 to 10.

13. The process of claim 12 , further comprising a step (7) of drying the aqueous salt solution produced in step (5) or (6).

14. The process of claim 1 , further comprising a step (6) of drying the aqueous salt solution produced in step (5).

15. The process of claim 1 , wherein the aqueous salt solution further comprises calcium nitrate.

16. The process of claim 1 , wherein the acidic wastewater further comprises nitric acid.

17. The process of claim 10 , wherein the chelating sulfur containing groups of the scavenger resin comprise chelating thiourea groups.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 17, 2021
From: YU, ZHENGGANG; CHEN, LI
To: HERAEUS PRECIOUS METAL TECHNOLOGY (CHINA) CO., LTD.
Reel/Frame 056258/0850 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 12, 2019
From: NOWOTTNY, CHRISTIAN
To: HERAEUS SITE OPERATIONS GMBH & CO. KG
Reel/Frame 050362/0823 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 12, 2019
From: LEHR, BIRGER; JANITZ, HARTMUT
To: HERAEUS DEUTSCHLAND GMBH & CO. KG
Reel/Frame 050362/0877 →
Continuity (1)
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