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US4572824A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for recovery of zirconium and acid from spent etching solutions

Assignee: General Electric Co
•
Filing: 1984-11-01
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Granted: 1986-02-25
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Expires: 2004-11-01
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Abstract

Abstract In the manufacture of nuclear fuel tubes spent etching solutions containing nitric acid, zirconium, and hydrofluoric acid are produced as waste. A serial treatment process is employed to recover the zirconium and to restore the solution to the desired acid concentration. These processes include solvent extraction for zirconium removal and aqueous removal using evaporation or distillation.

Inventors

  • 👤 Bang M. Kim

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 08:35
CPC Classifications
C; C23; C23F; C23F1/00; C23F1/46; C01; C01G; C01G25/00; C01G25/003

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 151 words
A method for treating spent aqueous etchant containing zirconium, nitric acid, and hydrofluoric acid from a zirconium tube etching bath, said method comprising: contacting said zirconium bearing etchant solution with a first side of a first membrane disposed in a first chamber to produce zirconium depleted etchant; contacting the second side of said first membrane with a zirconium selective solvent; circulating said solvent which has been in contact with said second side of said first membrane in said first chamber so as to contact a first side of a second membrane disposed in a second chamber; recirculating the solvent which has been in contact with the first side of said second membrane so as to recontact the second side of said first membrane contacting the second side of said second membrane with a stripping solution; and removing water from said zirconium depleted etchant whereby the concentration of said acids is increased
Claim 2
Independent Claim 151 words
A method for treating spent aqueous etchant containing zirconium, nitric acid, and hydrofluoric acid from a zirconium tube etching bath, said method comprising: contacting said zirconium bearing etchant solution with a first side of a first membrane disposed in a first chamber to produce zirconium depleted etchant; contacting the second side of said first membrane with a zirconium selective solvent; circulating said solvent which has been in contact with said second side of said first membrane in said first chamber so as to contact a first side of a second membrane disposed in a second chamber; recirculating the solvent which has been in contact with the first side of said second membrane so as to recontact the second side of said first membrane contacting the second side of said second membrane with a stripping solution; and removing water from said zirconium depleted etchant whereby the concentration of said acids is increased
Claim 3
Dependent Claim 11 words
The method of claim 1 in which said solvent comprises DEHPA.
Claim 4
Dependent Claim 26 words
The method of claim 1 in which said solvent comprises a solution comprising DEHPA and material selected from the group consisting of kerosene and aromatic hydrocarbons.
Claim 5
Dependent Claim 27 words
The method of claim 1 in which said membrane based extractor process employs a stripping agent selected from the group consisting of hydrofluoric acid and ammonium fluoride.
Claim 6
Dependent Claim 24 words
The method of claim 4 in which the concentration of said stripping agent in an aqueous solution is between about 0.5 and 3 mole/liter.
Claim 7
Dependent Claim 14 words
The method of claim 1 in which said water removal is performed by evaporation.
Claim 8
Dependent Claim 14 words
The method of claim 1 in which said water removal is performed by distillation.
Claim 9
Dependent Claim 21 words
The method of claim 1 further including the step of returning said solution with concentrated nitric acid to said etching bath.

References Cited (Backward Citations)

US3788915A Cited
US3956112A Cited
US4233108A Cited
US3957504A Cited
US4200612A Cited
US4252602A Cited
US4443414A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1989-02-24 1989-08-26 1990-02-25 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1993-02-24 1993-08-26 1994-02-25 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1997-02-24 1997-08-26 1998-02-25 $7700.00 Window Closed / Lapsed

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