US4200612A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for recovering acids and zirconium contained in pickling solutions
Assignee: Ugine Aciers SA
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Filing: 1978-11-07
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Granted: 1980-04-29
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Expires: 1998-11-07
Abstract
Abstract A process for recovery of zirconium from pickling solutions which have been used to treat products formed of zirconium or zirconium-based alloys, the invention particularly provides for separating zirconium from the acids contained in such solutions. The present process comprises passing the used or spent pickling solutions which contain from 1 to 50 g/l of dissolved zirconium through a column of an anionic ion-exchange resin by means of which the zirconium ions are separated from fluoride and nitrate ions originally present in the pickling solutions. Approximately 90% of the zirconium contained in such solutions can be recovered according to the invention, it being further possible to recycle residual fluoride and nitrate ions which remain in the used pickling solutions.
Inventors
- 👤 Airy P. Lamaze
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 09:40
CPC Classifications
C; C23; C23G; C23G1/00; C23G1/36; B; B01; B01J; B01J41/00; B01J41/04; B01J49/00; B01J49/05; B01J49/07; C01; C01G; C01G25/00; C01G25/003; C01G25/06; C22; C22B; C22B3/00; C22B3/20; C22B3/42; C23F; C23F1/00; C23F1/46; Y; Y02; Y02P; Y02P10/00; Y02P10/20
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
136 words
A process for recovering zirconium values from a pickling solution containing fluoride and nitrate ions, comprising the steps of: preparing an anionic ion exchange resin in a column with a sulfuric acid solution in order to saturate the resin with sulfate ions; contacting the resin thus prepared with a used pickling solution containing zirconium in a concentration of less than 50 grams per liter of solution and also containing fluoride and nitrate ions, the zirconium being absorbed by the resin; and, passing a hydrochloric acid solution through the column to replace the used pickling solution containing fluoride and nitrate ions and, on volumetric displacement of the used pickling solution, continuing to pass the hydrochloric acid solution through the column to elute zirconium from the column in a sulfate solution separately from the replaced used pickling solution.
Claim 2
Dependent Claim
136 words
A process for recovering zirconium values from a pickling solution containing fluoride and nitrate ions, comprising the steps of: preparing an anionic ion exchange resin in a column with a sulfuric acid solution in order to saturate the resin with sulfate ions; contacting the resin thus prepared with a used pickling solution containing zirconium in a concentration of less than 50 grams per liter of solution and also containing fluoride and nitrate ions, the zirconium being absorbed by the resin; and, passing a hydrochloric acid solution through the column to replace the used pickling solution containing fluoride and nitrate ions and, on volumetric displacement of the used pickling solution, continuing to pass the hydrochloric acid solution through the column to elute zirconium from the column in a sulfate solution separately from the replaced used pickling solution.
Claim 3
Dependent Claim
30 words
The process of claim 1 wherein the preparing step comprises: passing a sulfuric acid solution through the column; and, rinsing the column with distilled water to remove excess sulfuric acid.
Claim 4
Dependent Claim
14 words
The process of claim 2 wherein the sulfuric acid solution is approximately 1 N.
Claim 5
Dependent Claim
53 words
The process of claim 1 wherein nitrate ion is present in the used pickling solution in the acid form in a concentration of between 2 and 5 N and wherein the fluoride ion is present in the used pickling solution in the acid form in a concentration of between 0.5 and 2 N.
Claim 6
Dependent Claim
22 words
The process of claim 1 wherein zirconium is present in the used pickling solution in a concentration of less than 25 g/l.
Claim 7
Dependent Claim
21 words
The process of claim 1 wherein zirconium is present in the used pickling solution in a concentration greater than 1.0 g/l.
Claim 8
Dependent Claim
14 words
The process of claim 1 wherein the hydrochloric acid solution is approximately 1 N.
Claim 9
Dependent Claim
24 words
The process of claim 1 wherein the used pickling solution is passed through the column at a rate of approximately 2 liters per hour.
References Cited (Backward Citations)
US2567661A
Cited
BE672649A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1983-04-29 | 1983-10-29 | 1984-04-29 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1987-04-29 | 1987-10-29 | 1988-04-29 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1991-04-29 | 1991-10-29 | 1992-04-29 | $7700.00 | Window Closed / Lapsed |