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US4118219A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for recycling junk lead-acid batteries

Assignee: GNB Inc
•
Filing: 1977-07-01
•
Granted: 1978-10-03
•
Expires: 1997-07-01
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Abstract

Abstract A hydrometallurgical process for recycling the paste and electrolyte of junk lead-acid batteries begins by separating the paste and electrolyte from the junk batteries. The paste and electrolyte are then reacted to increase the lead sulfate content of the paste and reduce the acid content of the electrolyte. Excess liquid is then removed from the mixture of paste and electrolyte, after which the paste is mixed with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead sulfate from the paste. The remaining solid materials are then separated from the resulting pregnant lead solution, after which lead carbonate is precipitated from the pregnant lead solution by the addition of ammonium carbonate, ammonium bicarbonate or carbon dioxide. The precipitated lead carbonate is removed from the spent liquid and either converted to lead oxide by calcining, or mixed with sulfuric acid and then calcined or reacted with a chemical reducing agent to convert lead dioxide therein to lead oxide, and the lead oxide-containing material is then mixed with sulfuric acid in a second sulfating reaction to increase the lead sulfate content thereof. The resulting product is mixed with an aqueous ammoniacal ammonium sulfate solution to dissolve further lead sulfate therefrom. The resulting pregnant lead solution is separated from any solid materials remaining therein, after which lead carbonate is precipitated from the solution.

Inventors

  • 👤 Marion Edward Elmore
  • 👤 James Kenneth Klang

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 14:07
CPC Classifications
H; H01; H01M; H01M10/00; H01M10/54; Y; Y02; Y02W; Y02W30/00; Y02W30/50; Y02W30/84

Claims Analysis

Total Claims: 38
Claim 1
Independent Claim 97 words
A process for recycling the paste and electrolyte of junk lead-acid batteries, said process comprising the steps of (a) separating the paste and electrolyte from the junk batteries, (b) reacting the paste and electrolyte to increase the lead sulfate content of the paste and reduce the acid content of the electrolyte, (c) mixing the resulting paste with an aqueous ammoniacal ammonium sulfae solution to dissolve a substantial portion of the lead sulfate from the paste, (d) separating the resulting pregnant lead solution from any solid materials therein, (e) and precipitating lead carbonate from the pregnant lead solution.
Claim 2
Dependent Claim 97 words
A process for recycling the paste and electrolyte of junk lead-acid batteries, said process comprising the steps of (a) separating the paste and electrolyte from the junk batteries, (b) reacting the paste and electrolyte to increase the lead sulfate content of the paste and reduce the acid content of the electrolyte, (c) mixing the resulting paste with an aqueous ammoniacal ammonium sulfae solution to dissolve a substantial portion of the lead sulfate from the paste, (d) separating the resulting pregnant lead solution from any solid materials therein, (e) and precipitating lead carbonate from the pregnant lead solution.
Claim 3
Dependent Claim 56 words
The process of claim 1 wherein said electrolyte contains an insufficient amount of sulfuric acid to react with all the lead oxide in said paste, and additional sulfuric acid is added to the mixture of paste and electrolyte to react with the excess lead oxide and thereby further increase the lead sulfate content of the paste.
Claim 4
Dependent Claim 29 words
The process of claim 1 wherein excess liquid is removed from the mixture of paste and electrolyte prior to mixing the paste with the aqueous ammoniacal ammonium sulfate solution.
Claim 5
Dependent Claim 22 words
The process of claim 1 wherein lead dioxide in the paste is converted to lead oxide prior to mixing with the electrolyte.
Claim 6
Dependent Claim 18 words
The process of claim 4 wherein said paste is calcined to convert the lead dioxide to lead oxide.
Claim 7
Dependent Claim 23 words
The process of claim 4 wherein a chemical reducing agent is added to the paste to convert the lead dioxide to lead oxide.
Claim 8
Dependent Claim 19 words
The process of claim 6 wherein said paste is ground before the addition of said chemical reducing agent thereto.
Claim 9
Dependent Claim 21 words
The process of claim 1 wherein the precipitated lead carbonate is removed from the mother liquor and converted to lead oxide.
Claim 10
Dependent Claim 23 words
The process of claim 1 wherein the precipitated lead carbonate is mixed with sulfuric acid and then calcined to produce basic lead sulfates.
Claim 11
Dependent Claim 24 words
The process of claim 1 wherein the precipitated lead carbonate is fed to a reduction furnace where it is converted to substantially pure lead.
Claim 12
Dependent Claim 62 words
The process of claim 1 which includes the steps of converting lead dioxide to lead oxide in the solid materials separated from the pregnant lead solution, mixing the resulting materials with sulfuric acid to increase the lead sulfate content thereof, and mixing the resulting product with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead sulfate therefrom.
Claim 13
Dependent Claim 25 words
The process of claim 11 wherein said solid materials separated from the pregnant lead solution are calcined to convert the lead dioxide to lead oxide.
Claim 14
Dependent Claim 30 words
The process of claim 11 wherein a chemical reducing agent is added to said solid materials separated from the pregnant lead solution to convert the lead dioxide to lead oxide.
Claim 15
Dependent Claim 20 words
The process of claim 13 wherein said solid materials are ground before the addition of said chemical reducing agent thereto.
Claim 16
Dependent Claim 31 words
The process of claim 11 which includes the steps of separating the resulting pregnant lead solution from any solid materials remaining therein, and precipitating lead carbonate from the pregnant lead solution.
Claim 17
Dependent Claim 21 words
The process of claim 1 wherein ammonium sulfate is removed from the solution from which the lead carbonate has been precipitated.
Claim 18
Dependent Claim 30 words
The process of claim 1 wherein at least a portion of the solution from which the lead carbonate has been precipitated is recycled to the aqueous ammoniacal ammonium sulfate solution.
Claim 19
Dependent Claim 16 words
The process of claim 17 wherein ammonia and ammonium sulfate are added to the recycled solution.
Claim 20
Dependent Claim 92 words
A process for recycling the paste of junk lead-acid batteries, said process comprising the steps of (a) reacting the paste from the junk batteries with sulfuric acid to convert lead oxide therein to lead sulfate and thereby increase the lead sulfate content of the paste, (b) mixing the resulting paste with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead sulfate from the paste, (c) separating the resulting pregnant lead solution from any solid materials remaining therein, (d) and precipitating lead carbonate from the pregnant lead solution.
Claim 21
Dependent Claim 92 words
A process for recycling the paste of junk lead-acid batteries, said process comprising the steps of (a) reacting the paste from the junk batteries with sulfuric acid to convert lead oxide therein to lead sulfate and thereby increase the lead sulfate content of the paste, (b) mixing the resulting paste with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead sulfate from the paste, (c) separating the resulting pregnant lead solution from any solid materials remaining therein, (d) and precipitating lead carbonate from the pregnant lead solution.
Claim 22
Dependent Claim 91 words
A process for recovering lead from junk lead-acid batteries comprising the steps of (a) removing all the internal components of the batteries, including the acid, from the battery cases and mixing said internal components together to convert lead oxide therein to lead sulfate, (b) adding ammoniacal ammonium sulfate to said mixture to leach the lead from said mixture, (c) precipitating lead carbonate from the resulting solution and removing the precipitate from the solution, (d) and converting the lead carbonate to lead oxide by the removal of carbon dioxide from the carbonate.
Claim 23
Dependent Claim 91 words
A process for recovering lead from junk lead-acid batteries comprising the steps of (a) removing all the internal components of the batteries, including the acid, from the battery cases and mixing said internal components together to convert lead oxide therein to lead sulfate, (b) adding ammoniacal ammonium sulfate to said mixture to leach the lead from said mixture, (c) precipitating lead carbonate from the resulting solution and removing the precipitate from the solution, (d) and converting the lead carbonate to lead oxide by the removal of carbon dioxide from the carbonate.
Claim 24
Dependent Claim 93 words
A process for recovering lead from junk lead-acid batteries comprising the steps of (a) removing all the internal components of the batteries, including the acid, from the battery cases and mixing said internal components together to convert lead oxide therein to lead sulfate, (b) adding ammoniacal ammonium sulfate to said mixture to leach the lead from said mixture, (c) precipitating lead carbonate from the resulting solution and removing the precipitate from the solution, (d) and mixing the lead carbonate with sulfuric acid and then calcining the resulting mixture to produce basic lead sulfates.
Claim 25
Dependent Claim 93 words
A process for recovering lead from junk lead-acid batteries comprising the steps of (a) removing all the internal components of the batteries, including the acid, from the battery cases and mixing said internal components together to convert lead oxide therein to lead sulfate, (b) adding ammoniacal ammonium sulfate to said mixture to leach the lead from said mixture, (c) precipitating lead carbonate from the resulting solution and removing the precipitate from the solution, (d) and mixing the lead carbonate with sulfuric acid and then calcining the resulting mixture to produce basic lead sulfates.
Claim 26
Dependent Claim 87 words
A process for recovering lead from junk lead-acid batteries comprising the steps of (a) removing all the internal components of the batteries, including the acid, from the battery cases and mixing said internal components together to convert lead oxide therein to lead sulfate, (b) adding ammoniacal ammonium sulfate to said mixture to leach the lead from said mixture, (c) precipitating lead carbonate from the resulting solution and removing the precipitate from the solution, (d) and converting the lead carbonate to substantially pure lead in a reduction furnace.
Claim 27
Dependent Claim 87 words
A process for recovering lead from junk lead-acid batteries comprising the steps of (a) removing all the internal components of the batteries, including the acid, from the battery cases and mixing said internal components together to convert lead oxide therein to lead sulfate, (b) adding ammoniacal ammonium sulfate to said mixture to leach the lead from said mixture, (c) precipitating lead carbonate from the resulting solution and removing the precipitate from the solution, (d) and converting the lead carbonate to substantially pure lead in a reduction furnace.
Claim 28
Dependent Claim 88 words
A process for recycling the paste from junk lead-acid batteries, said process comprising the steps of (a) separating a paste containing lead dioxide from the junk batteries, (b) converting the lead dioxide in the paste to a form of lead that is soluble in an aqueous ammoniacal ammonium sulfate solution. (c) mixing the resulting soluble lead product with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead from said soluble lead product, (d) and removing the lead from the resulting pregnant lead solution.
Claim 29
Dependent Claim 88 words
A process for recycling the paste from junk lead-acid batteries, said process comprising the steps of (a) separating a paste containing lead dioxide from the junk batteries, (b) converting the lead dioxide in the paste to a form of lead that is soluble in an aqueous ammoniacal ammonium sulfate solution. (c) mixing the resulting soluble lead product with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead from said soluble lead product, (d) and removing the lead from the resulting pregnant lead solution.
Claim 30
Dependent Claim 28 words
The process of claim 23 wherein said lead dioxide is converted to lead oxide by calcining the paste, and said lead oxide is then converted to lead sulfate.
Claim 31
Dependent Claim 33 words
The process of claim 23 wherein said lead dioxide is converted to lead oxide by adding a chemical reducing agent to the paste, and said lead oxide is then converted to lead sulfate.
Claim 32
Dependent Claim 18 words
The process of claim 25 wherein the paste is ground before the addition of the chemical reducing agent.
Claim 33
Dependent Claim 35 words
The process of claim 23 wherein said lead dioxide is converted to lead oxide, and said lead oxide is then converted to lead sulfate by reacting the paste with electrolyte separated from the junk batteries.
Claim 34
Dependent Claim 34 words
The process of claim 23 wherein the lead is removed from said pregnant lead solution by separating said solution from any solid materials therein, and then precipitating lead carbonate from the pregnant lead solution.
Claim 35
Dependent Claim 94 words
A process for recycling the paste from junk lead-acid batteries, said process comprising the steps of (a) separating a paste containing lead sulfate, lead oxide and lead dioxide from the junk batteries, (b) converting the lead dioxide in the paste to lead oxide, (c) reacting the paste with sulfuric acid to convert the lead oxide therein to lead sulfate, (d) mixing the resulting paste with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead sulfate from the paste, (e) and removing the lead from the resulting pregnant lead solution.
Claim 36
Dependent Claim 94 words
A process for recycling the paste from junk lead-acid batteries, said process comprising the steps of (a) separating a paste containing lead sulfate, lead oxide and lead dioxide from the junk batteries, (b) converting the lead dioxide in the paste to lead oxide, (c) reacting the paste with sulfuric acid to convert the lead oxide therein to lead sulfate, (d) mixing the resulting paste with an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the lead sulfate from the paste, (e) and removing the lead from the resulting pregnant lead solution.
Claim 37
Dependent Claim 88 words
Lead oxide produced by reacting the paste from junk batteries with sulfuric acid to convert lead oxide therein to lead sulfate, mixing the resulting paste wiith an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the land sulfate from the paste, separating the resulting pregnant lead solution from any solid materials remaining therein, precipitating lead carbonate from the pregnant lead solution and removing the precipitate from the solution, and converting the lead carbonate to lead oxide by the removal of carbon dioxide from the carbonate.
Claim 38
Dependent Claim 88 words
Lead oxide produced by reacting the paste from junk batteries with sulfuric acid to convert lead oxide therein to lead sulfate, mixing the resulting paste wiith an aqueous ammoniacal ammonium sulfate solution to dissolve a substantial portion of the land sulfate from the paste, separating the resulting pregnant lead solution from any solid materials remaining therein, precipitating lead carbonate from the pregnant lead solution and removing the precipitate from the solution, and converting the lead carbonate to lead oxide by the removal of carbon dioxide from the carbonate.

References Cited (Backward Citations)

US1148062A Cited
US1570438A Cited
US2104076A Cited
US2328089A Cited
US3440155A Cited
US3883348A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-10-02 1982-04-03 1982-10-03 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-10-02 1986-04-03 1986-10-03 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-10-02 1990-04-03 1990-10-03 $7700.00 Window Closed / Lapsed

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