IP Library Granted Patent US 11,254,585
Granted Patent B2
US 11,254,585 · App. 17/126,254 · Granted Feb 22, 2022

Method for treating pickling acid residue

Inventors: Kenneth Ekman (Harjavalta, FI); Peik Ekman (Harjavalta, FI); Elina Lappalainen (Harjavalta, FI)
Assignee: CrisolteQ Ltd
C01G53/10C01F5/40C01G53/003C22B7/006C22B23/04
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Quick Facts
Patent No.
US 11,254,585
App. No.
17/126,254
Granted
Feb 22, 2022
Kind
B2
Abstract

A novel process for treating pickling acid residue and recovering sulfates and nickel therefrom has been developed. By lowering the pH of a magnesium compound slurry to 4-5.5 with sulfuric acid containing pickling acid residue in the presence of ammonium sulfate, both magnesium sulfate and nickel sulfate are solubilized. Magnesium sulfate and nickel sulfate solution is separated from the solids by filtration and an iron hydroxide and chromium hydroxide residue is obtained as a precipitate. Magnesium sulfate and nickel sulfate are then separated from the solution.

Claims (14)

1. A method for recovering sulfates and nickel from a sulfuric acid containing pickling acid residue comprising the steps of:

slurrying under continuous stirring at least one magnesium compound selected from the group consisting of magnesium oxide, magnesium hydroxide, magnesium carbonate, and combinations thereof into water;

adding sulfuric acid containing pickling acid residue (PAR) under continuous stirring to obtain a Mg/PAR-slurry with a stable pH of 4-5.5 at a temperature between 70° C. and 90° C.;

continuing continuous stirring of the obtained Mg/PAR-slurry for at least 30 minutes at the temperature between 70° C. and 90° C.;

adding ammonium sulfate at any stage before filtration of the obtained Mg/PAR-slurry;

separating an iron and chromium-containing residue by filtration and obtaining a solution of nickel sulfate and magnesium sulfate as a filtrate; and

recovering sulfates and nickel from the nickel sulfate and magnesium sulfate solution filtrate.

2. The method for recovering according to claim 1 , wherein the sulfates are recovered as magnesium sulfate solution by separating the nickel from the nickel sulfate and magnesium sulfate solution filtrate by adsorbing nickel on an ion exchange resin and nickel is recovered as nickel sulfate from the ion exchange resin by elution with sulfuric acid.

3. The method for recovering according to claim 1 , wherein the magnesium compound is magnesium oxide.

4. The method for recovering according to claim 1 , wherein the magnesium compound is magnesium hydroxide.

5. The method for recovering according to claim 1 , wherein the magnesium compound is magnesium carbonate.

6. The method for recovering according to claim 1 , wherein the magnesium compound is a combination of magnesium oxide, magnesium hydroxide, and magnesium carbonate.

7. The method for recovering according to claim 1 , wherein the at least one magnesium compound is added in dry form.

8. The method for recovering according to claim 1 , wherein the concentration of the ammonium sulfate in the Mg/PAR-slurry is between 0.5 and 5% (w/V).

Assignments (2)
CHANGE OF NAME Recorded Jun 8, 2023
From: CRISOLTEQ LTD
To: FORTUM BATTERY RECYCLING OY
Reel/Frame 063915/0774 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 18, 2021
From: EKMAN, KENNETH; EKMAN, PEIK; LAPPALAINEN, ELINA
To: CRISOLTEQ LTD
Reel/Frame 055635/0321 →
Priority Claims (1)
FI 20196110 · Dec 19, 2019 · national
Continuity (1)
Related Publication 20210188659A1 · Jun 24, 2021
Cited By (5)
US 12,195,338 US 12,214,420 US 12,261,023 US 12,311,447 US 12,406,829