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US3877931A Expired / Lapsed US ⏱️ 0.0 years remaining

Continuous preparation of pure metals by gaseous reduction

Assignee: Individual
•
Filing: 1974-05-13
•
Granted: 1975-04-15
•
Expires: 1994-05-13
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Abstract

Abstract A process for continuously recovering metal powders of high purity from aqueous solutions of the salts thereof which comprises conditioning the aqueous solution to attain a selected free ammonia to metal mole ratio in the general range of from 0.0:1 to about 6:1, depending upon the solution used and the metal to be reduced, then continuously passing the solution through a tubular reactor under steady state conditions in modified plug flow in which localized, limited backmixing occurs, while continuously charging a reducing gas to the reactor in countercurrent flow with respect to the solution to agitate the solution as it passes through the reactor, and to continuously reduce selected metal ions to yield insoluble metal powder. A temperature gradient is preferably maintained over at least a portion of the length of the tubular reactor from ambient temperature at the point of charging the leach solution to a temperature preferably exceeding 200*F at a location spaced from the ambient temperature point.

Inventors

  • 👤 Daniel R Neskora
  • 👤 Cedomir M Sliepcevich
  • 👤 Robert L Brown

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 15:53
CPC Classifications
C; C22; C22B; C22B23/00; C22B23/04; C22B23/0453; C22B23/0461; B; B01; B01J; B01J19/00; B01J19/24; B01J19/2415; C22B15/00; C22B15/0063; C22B3/00; C22B3/20; C22B3/44; C22B5/00; C22B5/02; C22B5/12; B01J2219/00; B01J2219/00049; B01J2219/00051; B01J2219/00074; B01J2219/00087; B01J2219/00094; B01J2219/18; B01J2219/185; B01J2219/19; B01J2219/194; B01J2219/1941; B01J2219/1943; Y; Y02; Y02P; Y02P10/00; Y02P10/20

Claims Analysis

Total Claims: 13
Claim 1
Independent Claim 285 words
IN A PROCESS FOR CONTINUOUSLY RECOVERING METALLIC COPPER, NICKEL, COBALT, SILVER OR GOLD FROM AN AQUEOUS SOLUTION CONTAINING A SOLUBLE SALT OF ONE OR MORE OF THESE METALS, AND HAVING A SELECTED PH AND A SELECTED FREE AMMONIA-TO-METAL RATIO RANGING FROM 0:1 UP TO ABOUT 6:1, DEPENDING UPON THE METAL TO BE RECOVERED, BY CONTINUOUSLY MIXING THE SOLUTION WITH A REDUCING GAS IN A TUBULAR REACTOR, THE IMPROVEMENT WHICH COMPRISES: CONTINUOUSLY CHARGING THE SOLUTION AND ANY NEEDED PARTICULATE CATALYST TO A TUBULAR REACTOR WHILE SIMULTANEOUSLY INTRODUCING A REDUCING GAS TO SAID REACTOR AT A POINT SPACED FROM THE POINT AT WHICH THE SOLUTION IS CHARGED TO THE REACTOR IN A FLOW DIRECTION CONTERCURRENT TO THE FLOW DIRECTION OF THE SOLUTION; HEATING THE MIXTURE OF THE SOLUTION AND THE GAS TO A TEMPERATURE OF AT LEAST 200*F PRIOR TO PASSING OUT OF THE REACTOR, SAID REACTOR BEING MAINTAINED, DURING THE CHARGING OF THE SOLUTION AND INTRODUCTION OF THE GAS, UNDER SUBSTANTIALLY STEADY STATE CONDITIONS IN WHICH A. THE PARTIAL PRESSURE OF THE REDUCING GAS IS AT LEAST 50 PSIG, AND THE TOTAL PRESSURE ON THE SOLUTION IS SUFFICIENT TO PREVENT BOILING OF THE SOLUTION; B. THE QUANTITY OF REDUCING GAS PASSED THROUGH THE REACTOR COUNTERCURRENTLY WITH THE AQUEOUS SOLUTION IS IN EXCESS OF THAT REQUIRED FOR STOICHIOMETRIC REDUCTION OF THE METAL VALUES TO BE RECOVERED AND IN SUFFICIENT QUANTITY AND FLOW RATE TO AGITATE THE MIXTURE TO A STATE OF MODIFIED PLUG FLOW IN WHICH LOCALIZED, LIMITED BACKMIXING OCCURS, AND IN WHICH C. THE MIXTURE IS OF HETEROGENEOUS CHARACTER OVER THE LENGTH AND THE REACTOR; THEN SEPARATING THE METAL POWDER TO BE RECOVERED FROM THE EFFLUENT MIXTURE OF SPENT SOLUTION AND SOILDS DISCHARGED FROM THE REACTOR.
Claim 2
Dependent Claim 285 words
IN A PROCESS FOR CONTINUOUSLY RECOVERING METALLIC COPPER, NICKEL, COBALT, SILVER OR GOLD FROM AN AQUEOUS SOLUTION CONTAINING A SOLUBLE SALT OF ONE OR MORE OF THESE METALS, AND HAVING A SELECTED PH AND A SELECTED FREE AMMONIA-TO-METAL RATIO RANGING FROM 0:1 UP TO ABOUT 6:1, DEPENDING UPON THE METAL TO BE RECOVERED, BY CONTINUOUSLY MIXING THE SOLUTION WITH A REDUCING GAS IN A TUBULAR REACTOR, THE IMPROVEMENT WHICH COMPRISES: CONTINUOUSLY CHARGING THE SOLUTION AND ANY NEEDED PARTICULATE CATALYST TO A TUBULAR REACTOR WHILE SIMULTANEOUSLY INTRODUCING A REDUCING GAS TO SAID REACTOR AT A POINT SPACED FROM THE POINT AT WHICH THE SOLUTION IS CHARGED TO THE REACTOR IN A FLOW DIRECTION CONTERCURRENT TO THE FLOW DIRECTION OF THE SOLUTION; HEATING THE MIXTURE OF THE SOLUTION AND THE GAS TO A TEMPERATURE OF AT LEAST 200*F PRIOR TO PASSING OUT OF THE REACTOR, SAID REACTOR BEING MAINTAINED, DURING THE CHARGING OF THE SOLUTION AND INTRODUCTION OF THE GAS, UNDER SUBSTANTIALLY STEADY STATE CONDITIONS IN WHICH A. THE PARTIAL PRESSURE OF THE REDUCING GAS IS AT LEAST 50 PSIG, AND THE TOTAL PRESSURE ON THE SOLUTION IS SUFFICIENT TO PREVENT BOILING OF THE SOLUTION; B. THE QUANTITY OF REDUCING GAS PASSED THROUGH THE REACTOR COUNTERCURRENTLY WITH THE AQUEOUS SOLUTION IS IN EXCESS OF THAT REQUIRED FOR STOICHIOMETRIC REDUCTION OF THE METAL VALUES TO BE RECOVERED AND IN SUFFICIENT QUANTITY AND FLOW RATE TO AGITATE THE MIXTURE TO A STATE OF MODIFIED PLUG FLOW IN WHICH LOCALIZED, LIMITED BACKMIXING OCCURS, AND IN WHICH C. THE MIXTURE IS OF HETEROGENEOUS CHARACTER OVER THE LENGTH AND THE REACTOR; THEN SEPARATING THE METAL POWDER TO BE RECOVERED FROM THE EFFLUENT MIXTURE OF SPENT SOLUTION AND SOILDS DISCHARGED FROM THE REACTOR.
Claim 3
Dependent Claim 26 words
A process as defined in claim 1 wherein the reducing gas is selected from the group consisting of hydrogen, carbon monoxide, sulfur dioxide and hydrogen sulfide.
Claim 4
Dependent Claim 67 words
The process as defined in claim 1 wherein the aqueous solution is charged to the reactor at ambient temperature, and a constantly increasing thermal gradient is maintained in the reactor during its steady state operation from the first point therein at which the solution is charged to a second point therein spaced in the reactor toward the point of discharge of spent solution and product metal therefrom.
Claim 5
Dependent Claim 21 words
The process defined in claim 1 wherein the tubular reactor is operated isothermally over its length at a temperature exceeding 200*F.
Claim 6
Dependent Claim 19 words
The process defined in claim 1 wherein the reactor has a length to diameter ratio of at least 10:1.
Claim 7
Dependent Claim 35 words
The process defined in claim 1 wherein said reactor extends vertically, said solution is charged to the upper end of said reactor and said reducing gas is charged to the lower end of said reactor.
Claim 8
Dependent Claim 13 words
The process defined in claim 2 wherein the reducing gas employed is hydrogen.
Claim 9
Dependent Claim 38 words
The process defined in claim 4 wherein the maximum temperature in said thermal gradient is about half the distance from said first point to said point of discharge of said spent solution and product from said tubular reactor.
Claim 10
Dependent Claim 26 words
The process defined in claim 4 wherein the temperature at the point of discharge of spent solution and product from the reactor does not exceed 200*F.
Claim 11
Dependent Claim 33 words
The process defined in claim 8 wherein a constantly decreasing temperature gradient is maintained in the reactor from said second point to the point of discharge of spent solution and product metal therefrom.
Claim 12
Dependent Claim 38 words
A process as defined in claim 1 wherein said metal to be recovered is selected from the group consisting of copper, silver and gold, and the pH of the aqueous solution is adjusted to less than about 2.0.
Claim 13
Dependent Claim 76 words
A process as defined in claim 1 wherein the metal to be recovered is selected from the group consisting of nickel and cobalt, and wherein the pH of said aqueous solution is adjusted to from about 7 to about 12, and the free ammonia to metal ratio thereof is adjusted to from about 1.25:1 to about 6:1, and a catalyst for heterogeneous gaseous reduction of the metal to be recovered is added to said adjusted solution.

References Cited (Backward Citations)

US2753257A Cited
US2836485A Cited
US2867528A Cited
US3761250A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-04-14 1978-10-14 1979-04-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-04-14 1982-10-14 1983-04-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-04-14 1986-10-14 1987-04-15 $7700.00 Window Closed / Lapsed

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