Recycling of lead-containing waste

Patent metadata

Field	Value
Publication number	US-2022081315-A1
Application number	US-202017424875-A
Country	US
Kind code	A1
Filing date	Jan 21, 2020
Priority date	Jan 21, 2019
Publication date	Mar 17, 2022
Grant date	—

Abstract

A method for recycling lead-containing waste comprises: (a) dissolving the lead-containing waste in an aqueous solution of a first acid to form a solution of a first lead salt; (b) adding a second acid to the solution of the first lead salt to form a lead-depleted solution and a precipitate of a second lead salt; and (c) converting the precipitate of the second lead salt into leady oxide, wherein the first lead salt has a higher solubility in water than the second lead salt. The method may be used for recycling spent lead-acid battery paste.

First claim

1 . A method for recycling lead-containing waste, said method comprising:
(a) dissolving the lead-containing waste in an aqueous solution of a first acid to form a solution of a first lead salt; (b) adding a second acid to the solution of the first lead salt to form a lead-depleted solution and a precipitate of a second lead salt; and (c) converting the precipitate of the second lead salt into leady oxide, wherein the first lead salt has a higher solubility in water than the second lead salt.

2 . The method of claim 1 , wherein the lead-containing waste comprises at least one of Pb, PbO, PbCO 3 , or a combination thereof.

3 . The method of claim 1 , wherein the lead-containing waste is derived from lead-acid battery paste or from electric arc furnace dusts.

4 . The method of claim 1 , wherein:
the first lead salt has a solubility in water of at least 100 g/L; the second lead salt has a lower solubility in water than the first lead salt by at least 100 g/L; and/or the second lead salt has a solubility in water of up to 10 g/L.

5 . The method of claim 1 , wherein the first acid is an organic acid.

6 . The method of claim 1 , wherein lead-containing waste is dissolved in the aqueous solution of the first acid:
having a molarity of from 0.1 to 7 mol/L, preferably from 0.25 to 3 mol/L; in an amount of from 10 to 650 g of waste per litre of aqueous solution of the first acid; at a temperature of from 0 to 90° C.; at ambient pressure; for a time period of from 1 to 120 minutes; and/or under agitation.

7 . The method of claim 1 , wherein the lead-containing waste is contacted with a redox reagent chosen from hydrogen peroxide, metal hydrides, hydrogen gas, inorganic salts, and organic redox reagents.

8 . The method of claim 1 , wherein the lead-containing waste comprises material which is insoluble in the aqueous solution of the first acid and the method further comprises recovering said insoluble material from the solution of the first lead salt.

9 . The method of claim 8 , wherein the insoluble material comprises one or more of metal compounds chosen from barium sulfate; carbon compounds; and fibres.

10 . The method of claim 1 , wherein the second acid is an organic acid.

11 . The method of claim 1 , wherein the second acid is added to the solution of the first lead salt:
in an amount of from 60 to 100% of the stoichiometric amount required for the formation of the second lead salt; at a temperature of from −10 to 80° C.; at ambient pressure; for a time period of from 2 to 120 minutes; and/or under agitation.

12 . The method of claim 1 , wherein the precipitate of the second lead salt is separated from the lead-depleted solution.

13 . The method of claim 12 , wherein the lead-depleted solution is recycled and used as the aqueous solution of the first acid in step (a).

14 . The method of claim 1 , wherein the lead-depleted solution comprises residual lead.

15 . The method of claim 1 , wherein the precipitate of the second lead salt is converted into leady oxide by calcination.

16 . The method of claim 15 , wherein calcination takes place:
at a temperature of from 250 to 1000° C.; at a partial pressure of oxygen of from 0.01 to 5 atm; and/or for a time period of from 10 minutes to 6 hours.

17 . The method of claim 1 , wherein the leady oxide comprises PbO and Pb in a total amount of at least 99% by weight.

18 . The method of claim 1 , wherein the method further comprises processing the leady oxide into battery plates, and optionally incorporating said battery plates into a lead-acid battery.

19 . The method of claim 1 , wherein the lead-containing waste that is used in step (a) is substantially free from PbSO 4 .

20 . The method of claim 1 , wherein the lead-containing waste comprises PbSO 4 , and the method further comprises a pre-treatment step in which the lead-containing waste is desulfurised before it is used in step (a).

21 . The method of claim 20 , wherein the pre-treatment step comprises contacting the lead-containing waste with:
a base in an amount of from 1.5 to 3 moles of base per mole of lead sulfate in the lead-containing waste; or a carbonate in an amount of from 0.75 to 1.5 moles per mole of lead sulfate in the lead-containing waste.

22 . The method of claim 20 , wherein the method comprises monitoring the pre-treatment step until the content of PbSO 4 in the lead-containing waste is reduced to a target level of up to 500 ppm by weight.

23 . The method of claim 22 , wherein the monitoring of the pre-treatment step is carried out indirectly by monitoring a parameter which correlates with the amount of PbSO 4 in the lead-containing waste.

24 . A leady oxide material obtainable by the method of claim 1 .

25 . A battery plate comprising, or a lead-acid battery incorporating a battery plate which comprises the leady oxide material of claim 24 .

Assignees

• Aurelius Env Ltd
• Cambridge Entpr Ltd

Inventors

• Fox Athan Lucian
• Yiao Marcel
• Kumar Ramachandran Vasant
• Liu Rob
• Selvaraj Vimalnath

Classifications

• C22B3/22

  by physical processes, e.g. by filtration, by magnetic means {, or by thermal decomposition} (treatment or purification of solutions by liquid-liquid extraction C22B3/26) · CPC title

• C22B1/005

  Preliminary treatment of scrap (C22B1/02 - C22B1/26 take precedence) · CPC title

• C22B3/44

  by chemical processes (treatment or purification of solutions by liquid-liquid extraction C22B3/26, by ion-exchange extraction C22B3/42) · CPC title

• H01M4/16

  Processes of manufacture · CPC title

• C22B3/165

  with organic acids · CPC title