Patent US4041125A successfully refreshed from Google Patents.
US4041125A
Expired / Lapsed
US
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Process for separation of the lanthanides
Assignee: Forskningsgruppe for Sjeldne Jordarter
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Filing: 1976-05-19
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Granted: 1977-08-09
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Expires: 1996-05-19
Abstract
Abstract An improved liquid-liquid extraction process for the separation of the elements of the lanthanide series is disclosed. The process involves dissolving the lanthanides in a sulfuric acid solution to form rare earth sulfates whereafter the solution is contacted with an organic solvent immiscible with water and containing di (2-ethylhexyl) phosphoric acid whereby the lanthanides are separated from impurities and at least some of the lanthanides are extracted into the organic phase. Thereafter, the organic and aqueous phases are separated and the organic phase containing the impurities-separated lanthanides is subjected to a back extraction with an aqueous phase comprising an aqueous solution with sulfuric acid. The contact time between the aqueous and organic phases in the back extraction is regulated so that a desired or desired elements of the lanthanides are back extracted into the aqueous phase. The contact time is controlled and is less than the total extraction equilibrium time between the phases. The organic and aqueous solution concentrations are also controlled. After a predetermined contact time, the aqueous and organic phases are immediately separated.
Inventors
- 👤 Jorolf Alstad
- 👤 Leif Farbu
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 18:26
CPC Classifications
C; C01; C01F; C01F17/00; C01F17/20; C01F17/282; C01F17/10; C01F17/17; C22; C22B; C22B3/00; C22B3/20; C22B3/26; C22B3/38; C22B3/384; C22B3/3846; Y; Y02; Y02P; Y02P10/00; Y02P10/20
Claims Analysis
Total Claims: 6
Claim 1
Independent Claim
234 words
A liquid-liquid extraction process for the separation of yttrium from terbium comprising: a. admixing a mixture of rare earth elements including at least yttrium and terbium and impurities in aqueous solution with sulfuric acid to form an aqueous phase comprising an aqueous solution of rare earth sulfates including at least yttrium sulfate and terbium sulfate; b. contacting said aqueous phase with an organic phase comprising an organic solvent containing di(2-ethylhexyl) phosphoric acid, said organic solvent being substantially immiscible with water; c. maintaining the contact between the aqueous phase and the organic phase for a sufficient time so that substantially all of the yttrium and terbium are extracted into the organic phase; d. separating the aqueous phase from the organic phase; e. subjecting the separated organic phase of step (d) to a back extraction with an aqueous phase comprising an aqueous solution with sulfuric acid; f. regulating the time of contact between the separated organic phase and the back extraction aqueous phase to a period of less than the time to total extraction equilibrium for the phases and between the half time in minutes for the extraction of terbium from the separated organic phase into the back extraction aqueous phase and the half time in minutes for the extraction of yttrium from the separated organic phase into the back extraction aqueous phase; and g. separating the separated organic phase from the back extraction aqueous phase.
Claim 2
Dependent Claim
234 words
A liquid-liquid extraction process for the separation of yttrium from terbium comprising: a. admixing a mixture of rare earth elements including at least yttrium and terbium and impurities in aqueous solution with sulfuric acid to form an aqueous phase comprising an aqueous solution of rare earth sulfates including at least yttrium sulfate and terbium sulfate; b. contacting said aqueous phase with an organic phase comprising an organic solvent containing di(2-ethylhexyl) phosphoric acid, said organic solvent being substantially immiscible with water; c. maintaining the contact between the aqueous phase and the organic phase for a sufficient time so that substantially all of the yttrium and terbium are extracted into the organic phase; d. separating the aqueous phase from the organic phase; e. subjecting the separated organic phase of step (d) to a back extraction with an aqueous phase comprising an aqueous solution with sulfuric acid; f. regulating the time of contact between the separated organic phase and the back extraction aqueous phase to a period of less than the time to total extraction equilibrium for the phases and between the half time in minutes for the extraction of terbium from the separated organic phase into the back extraction aqueous phase and the half time in minutes for the extraction of yttrium from the separated organic phase into the back extraction aqueous phase; and g. separating the separated organic phase from the back extraction aqueous phase.
Claim 3
Dependent Claim
242 words
A liquid-liquid extraction process for the separation of yttrium from terbium comprising: a. admixing a mixture of rare earth elements including at least yttrium and terbium and impurities in aqueous solution 1.5 N with sulfuric acid to form an aqueous phase comprising an aqueous solution of rare earth sulfates including at least yttrium sulfate and terbium sulfate; b. contacting said aqueous phase with an organic phase comprising an organic solvent which is 1 M in di(2-ethylhexyl) phosphoric acid, said organic solvent being substantially immiscible with water; c. maintaining the contact between the aqueous phase and the organic phase for a sufficient time so that substantially all of the yttrium and terbium are extracted into the organic phase; d. separating the aqueous phase from the organic phase; e. subjecting the separated organic phase of step (d) to a back extraction with an aqueous phase comprising an aqueous solution 2.7 N with sulfuric acid; f. regulating the time of contact between the separated organic phase and the back extraction aqueous phase to a period of less than the time to total extraction equilibrium for the phases and between the half time in minutes for the extraction of terbium from the separated organic phase into the back extraction aqueous phase and the half time in minutes for the extraction of yttrium from the separated organic phase into the back extraction aqueous phase; and g. separating the separated organic phase from the back extraction aqueous phase.
Claim 4
Dependent Claim
242 words
A liquid-liquid extraction process for the separation of yttrium from terbium comprising: a. admixing a mixture of rare earth elements including at least yttrium and terbium and impurities in aqueous solution 1.5 N with sulfuric acid to form an aqueous phase comprising an aqueous solution of rare earth sulfates including at least yttrium sulfate and terbium sulfate; b. contacting said aqueous phase with an organic phase comprising an organic solvent which is 1 M in di(2-ethylhexyl) phosphoric acid, said organic solvent being substantially immiscible with water; c. maintaining the contact between the aqueous phase and the organic phase for a sufficient time so that substantially all of the yttrium and terbium are extracted into the organic phase; d. separating the aqueous phase from the organic phase; e. subjecting the separated organic phase of step (d) to a back extraction with an aqueous phase comprising an aqueous solution 2.7 N with sulfuric acid; f. regulating the time of contact between the separated organic phase and the back extraction aqueous phase to a period of less than the time to total extraction equilibrium for the phases and between the half time in minutes for the extraction of terbium from the separated organic phase into the back extraction aqueous phase and the half time in minutes for the extraction of yttrium from the separated organic phase into the back extraction aqueous phase; and g. separating the separated organic phase from the back extraction aqueous phase.
Claim 5
Dependent Claim
188 words
A liquid-liquid extraction process for the separation of yttrium from terbium comprising: a. admixing a mixture of rare earth elements including at least yttrium and terbium and impurities in aqueous solution 1.5 N with sulfuric acid to form an aqueous phase comprising an aqueous solution of rare earth sulfates including at least yttrium sulfate and terbium sulfate; b. contacting said aqueous phase with an organic phase comprising on organic solvent which is 1 M in di(2-ethylhexyl) phosphoric acid, said organic solvent being substantially immiscible with water; c. maintaining the contact between the aqueous phase and the organic phase for a sufficient time so that substantially all of the yttrium and terbium are extracted into the organic phase; d. separating the aqueous phase from the organic phase; e. subjecting the separated organic phase of item (d) to a back extraction with an aqueous phase comprising an aqueous solution 2.7 N with sulfuric acid; f. regulating the time of contact between the separated organic phase and the back extraction aqueous phase to a period of six minutes; and g. separating the separated organic phase from the back extraction aqueous phase.
Claim 6
Dependent Claim
188 words
A liquid-liquid extraction process for the separation of yttrium from terbium comprising: a. admixing a mixture of rare earth elements including at least yttrium and terbium and impurities in aqueous solution 1.5 N with sulfuric acid to form an aqueous phase comprising an aqueous solution of rare earth sulfates including at least yttrium sulfate and terbium sulfate; b. contacting said aqueous phase with an organic phase comprising on organic solvent which is 1 M in di(2-ethylhexyl) phosphoric acid, said organic solvent being substantially immiscible with water; c. maintaining the contact between the aqueous phase and the organic phase for a sufficient time so that substantially all of the yttrium and terbium are extracted into the organic phase; d. separating the aqueous phase from the organic phase; e. subjecting the separated organic phase of item (d) to a back extraction with an aqueous phase comprising an aqueous solution 2.7 N with sulfuric acid; f. regulating the time of contact between the separated organic phase and the back extraction aqueous phase to a period of six minutes; and g. separating the separated organic phase from the back extraction aqueous phase.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-08-08 | 1981-02-07 | 1981-08-09 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-08-08 | 1985-02-07 | 1985-08-09 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-08-08 | 1989-02-07 | 1989-08-09 | $7700.00 | Window Closed / Lapsed |