US4816233A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Ion exchange method for the recovery of scandium
Assignee: Osram Sylvania Inc
•
Filing: 1987-09-11
•
Granted: 1989-03-28
•
Expires: 2007-09-11
Abstract
Abstract A method of recovering quantitatively trace amounts of scandium from aqueous solutions containing large amounts of other metals consists of reducing any manganese and iron in the solution to the divalent states of manganese and iron. The solution is then adjusted to a pH from about 1.9 to about 2.1 and passed through a column of the ion exchange resin in the hydrogen form having an iminodiacetic acid functionality. The scandium is absorbed on the column and any base metals and rare earth metals which were also absorbed are removed by eluting with a dilute acid without removing the scandium. The scandium is subsequently removed from the column by eluting with a solution containing a chelating agent such as diglycolic acid. The scandium is then recovered from the solution by precipitation, filtering, washing, drying and calcined to the oxide.
Inventors
- 👤 William J. Rourke
- 👤 Wen-Chao Lai
- 👤 Samuel Natansohn
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 20:10
CPC Classifications
C; C22; C22B; C22B3/00; C22B3/20; C22B3/42; C01; C01F; C01F17/00; C01F17/10; C01F17/13; C01F17/20; C01F17/206; C01F17/212; F; F02; F02B; F02B75/00; F02B75/02; F02B2075/022; F02B2075/027; Y; Y02; Y02P; Y02P10/00; Y02P10/20; Y10; Y10S; Y10S423/00; Y10S423/09; Y10S423/14
Claims Analysis
Total Claims: 28
Claim 1
Independent Claim
330 words
A method of recovering scandium values from a tungsten ore residue comprising the following steps: Step 1 dissolving scandium contained in a tungsten ore residue comprising iron, manganese, and scandium with an acid solution containing a reducing agent to convert any dissolved tetravalent manganese to divalent manganese forming an acid solution comprising said scandium, iron, and divalent manganese; Step 2 converting any trivalent iron present in said acid solution comprising said scandium, iron, and divalent manganese from step 1 to divalent iron by adding an iron reducing agent forming a trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese; Step 3 adjusting said trivalent iron free solution comprising said scandium, divalent iron, and divalent manganese from step 2 to a pH from about 1.9 to about 2.1 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese; Step 4 removing said scandium contained in said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese from step 3 by contacting said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese with an ion exchange resin being in a hydrogen form and having an iminodiacetic acid functionality forming an ion exchange resin having said scandium absorbed thereon; Step 5 rinsing said ion exchange resin having said scandium absorbed thereon from step 4 with a dilute acid having a pH from about 1.9 to about 2.1 to remove any base metals and rare earth metals absorbed on said ion exchange resin without removing said scandium absorbed thereon; Step 6 eluting said scandium absorbed on said ion exchange resin with a solution comprising a chelating agent to form an elution solution comprising said scandium and said chelating agent; Step 7 precipitating said scandium from said elution solution comprising said scandium by adding a precipitating agent to said elution solution comprising said scandium to form a scandium precipitate in said elution solution; and Step 8 separating said scandium precipitate from said elution solution.
Claim 2
Independent Claim
330 words
A method of recovering scandium values from a tungsten ore residue comprising the following steps: Step 1 dissolving scandium contained in a tungsten ore residue comprising iron, manganese, and scandium with an acid solution containing a reducing agent to convert any dissolved tetravalent manganese to divalent manganese forming an acid solution comprising said scandium, iron, and divalent manganese; Step 2 converting any trivalent iron present in said acid solution comprising said scandium, iron, and divalent manganese from step 1 to divalent iron by adding an iron reducing agent forming a trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese; Step 3 adjusting said trivalent iron free solution comprising said scandium, divalent iron, and divalent manganese from step 2 to a pH from about 1.9 to about 2.1 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese; Step 4 removing said scandium contained in said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese from step 3 by contacting said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese with an ion exchange resin being in a hydrogen form and having an iminodiacetic acid functionality forming an ion exchange resin having said scandium absorbed thereon; Step 5 rinsing said ion exchange resin having said scandium absorbed thereon from step 4 with a dilute acid having a pH from about 1.9 to about 2.1 to remove any base metals and rare earth metals absorbed on said ion exchange resin without removing said scandium absorbed thereon; Step 6 eluting said scandium absorbed on said ion exchange resin with a solution comprising a chelating agent to form an elution solution comprising said scandium and said chelating agent; Step 7 precipitating said scandium from said elution solution comprising said scandium by adding a precipitating agent to said elution solution comprising said scandium to form a scandium precipitate in said elution solution; and Step 8 separating said scandium precipitate from said elution solution.
Claim 3
Dependent Claim
23 words
A method in accordance with claim 1 wherein said acid solution comprising a reducing agent in step 1 comprises hydrazine in sulfuric acid.
Claim 4
Dependent Claim
35 words
A method in accordance with claim 1 wherein said trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese in step 2 has a pH range from about 1.5 to about 1.7.
Claim 5
Dependent Claim
53 words
A method in accordance with claim 1 wherein said step 3 comprises adjusting said trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese from step 2 with a base to a pH of about 2.0 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese.
Claim 6
Dependent Claim
26 words
A method in accordance with claim 1 wherein said dilute acid of step 5 comprises a solution having a pH of about 1.9 to about 2.1.
Claim 7
Dependent Claim
38 words
A method in accordance with claim 1 wherein said chelating agent of said solution containing a chelating agent in step 6 is selected from the group consisting of diglycolic acid, carboxylic acid, hydroxy acid, EDTA, and combinations thereof.
Claim 8
Dependent Claim
24 words
A method in accordance with claim 1 wherein said chelating agent of said solution containing a chelating agent in step 6 is dyglycolic acid.
Claim 9
Dependent Claim
30 words
A method in accordance with claim 1 wherein step 7 comprises precipitating said scandium from said elution solution comprising said scandium with ammonium hydroxide to form a scandium hydroxide precipitate.
Claim 10
Independent Claim
326 words
A method of recovering scandium from an aqueous solution comprising scandium, iron, and manganese comprising the following steps: Step 1 adding acid and a reducing agent to an aqueous solution comprising scandium, iron, and manganese to convert any tetravalent manganese to divalent manganese forming an acid solution comprising said scandium, iron, and divalent manganese; Step 2 converting any trivalent iron present in said acid solution comprising said scandium, iron, and divalent manganese from step 1 to divalent iron by adding an iron reducing agent forming a trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese; Step 3 adjusting said trivalent iron free solution comprising said scandium, divalent iron, and divalent manganese from step 2 to a pH from about 1.9 to about 2.1 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese; Step 4 removing said scandium contained in said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese from step 3 by contacting said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese with an ion exchange resin being in a hydrogen form and having an iminodiacetic acid functionality forming an ion exchange resin having said scandium absorbed thereon; Step 5 rinsing said ion exchange resin having said scandium absorbed thereon from step 4 with a dilute acid having a pH from about 1.9 to about 2.1 to remove any base metals and rare earth metals absorbed on said ion exchange resin without removing said scandium absorbed thereon; Step 6 eluting said scandium absorbed on said ion exchange resin with a solution comprising a chelating agent to form an elution solution comprising said scandium and said chelating agent; Step 7 precipitating said scandium from said elution solution comprising said scandium by adding a precipitating agent to said elution solution comprising said scandium to form a scandium precipitate in said elution solution; and Step 8 separating said scandium precipitate from said elution solution.
Claim 11
Independent Claim
326 words
A method of recovering scandium from an aqueous solution comprising scandium, iron, and manganese comprising the following steps: Step 1 adding acid and a reducing agent to an aqueous solution comprising scandium, iron, and manganese to convert any tetravalent manganese to divalent manganese forming an acid solution comprising said scandium, iron, and divalent manganese; Step 2 converting any trivalent iron present in said acid solution comprising said scandium, iron, and divalent manganese from step 1 to divalent iron by adding an iron reducing agent forming a trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese; Step 3 adjusting said trivalent iron free solution comprising said scandium, divalent iron, and divalent manganese from step 2 to a pH from about 1.9 to about 2.1 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese; Step 4 removing said scandium contained in said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese from step 3 by contacting said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese with an ion exchange resin being in a hydrogen form and having an iminodiacetic acid functionality forming an ion exchange resin having said scandium absorbed thereon; Step 5 rinsing said ion exchange resin having said scandium absorbed thereon from step 4 with a dilute acid having a pH from about 1.9 to about 2.1 to remove any base metals and rare earth metals absorbed on said ion exchange resin without removing said scandium absorbed thereon; Step 6 eluting said scandium absorbed on said ion exchange resin with a solution comprising a chelating agent to form an elution solution comprising said scandium and said chelating agent; Step 7 precipitating said scandium from said elution solution comprising said scandium by adding a precipitating agent to said elution solution comprising said scandium to form a scandium precipitate in said elution solution; and Step 8 separating said scandium precipitate from said elution solution.
Claim 12
Dependent Claim
23 words
A method in accordance with claim 9 wherein said acid solution comprising a reducing agent in step 1 comprises hydrazine in sulfuric acid.
Claim 13
Dependent Claim
35 words
A method in accordance with claim 9 wherein said trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese in step 2 has a pH range from about 1.5 to about 1.7.
Claim 14
Dependent Claim
53 words
A method in accordance with claim 9 wherein said step 3 comprises adjusting said trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese from step 2 with a base to a pH of about 2.0 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese.
Claim 15
Dependent Claim
26 words
A method in accordance with claim 9 wherein said dilute acid of step 5 comprises a solution having a pH of about 1.9 to about 2.1.
Claim 16
Dependent Claim
38 words
A method in accordance with claim 9 wherein said chelating agent of said solution containing a chelating agent in step 6 is selected from the group consisting of diglycolic acid, carboxylic acid, hydroxy acid, EDTA, and combinations thereof.
Claim 17
Dependent Claim
24 words
A method in accordance with claim 9 wherein said chelating agent of said solution containing a chelating agent in step 6 is diglycolic acid.
Claim 18
Dependent Claim
30 words
A method in accordance with claim 9 wherein step 7 comprises precipitating said scandium from said elution solution comprising said scandium with ammonium hydroxide to form a scandium hydroxide precipitate.
Claim 19
Independent Claim
411 words
A method of recovering scandium from an aqueous solution comprising scandium, iron, and manganese comprising the following steps: Step 1 adding acid and a reducing agent to said aqueous solution comprising scandium, iron, and manganese to convert any tetravalent manganese to divalent manganese forming an acid solution comprising said scandium, iron, and divalent manganese; Step 2 converting any trivalent iron present in said acid solution comprising said scandium, iron, and divalent manganese from step 1 to divalent iron by adding an iron reducing agent forming a trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese; Step 3 adjusting said trivalent iron free solution comprising said scandium, divalent iron, and divalent manganese from step 2 to a pH from about 1.9 to about 2.1 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese; Step 4 removing said scandium contained in said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese from step 3 by contacting said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese with an ion exchange resin being in a hydrogen form and having an iminodiacetic acid functionality forming an ion exchange resin having said scandium absorbed thereon; Step 5 rinsing said ion exchange resin having said scandium absorbed thereon from step 4 with a dilute acid having a pH from about 1.9 to about 2.1 to remove any base metals and rare earth metals absorbed on said ion exchange resin without removing said scandium absorbed thereon; Step 6 eluting said scandium absorbed on said ion exchange resin with a solution comprising a chelating agent to form an elution solution comprising said scandium and said chelating agent; Step 7 removing said scandium from said elution solution comprising said scandium and said chelating agent by contacting said elution solution comprising said scandium and said chelating agent with a strong cation ion exchange resin being in a hydrogen form to form a strong cation ion exchange resin having said scandium absorbed thereon; Step 8 eluting said scandium absorbed on said strong cation exchange resin from step 7 with a strong acid to form a second acid solution comprising said scandium; Step 9 precipitating said scandium from said second acid solution comprising said scandium by adding a precipitating agent to said second acid solution comprising said scandium to form a scandium precipitate in a second acid solution; and Step 10 separating said scandium precipitate from said strong acid solution.
Claim 20
Independent Claim
411 words
A method of recovering scandium from an aqueous solution comprising scandium, iron, and manganese comprising the following steps: Step 1 adding acid and a reducing agent to said aqueous solution comprising scandium, iron, and manganese to convert any tetravalent manganese to divalent manganese forming an acid solution comprising said scandium, iron, and divalent manganese; Step 2 converting any trivalent iron present in said acid solution comprising said scandium, iron, and divalent manganese from step 1 to divalent iron by adding an iron reducing agent forming a trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese; Step 3 adjusting said trivalent iron free solution comprising said scandium, divalent iron, and divalent manganese from step 2 to a pH from about 1.9 to about 2.1 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese; Step 4 removing said scandium contained in said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese from step 3 by contacting said pH adjusted solution comprising said scandium, divalent iron, and divalent manganese with an ion exchange resin being in a hydrogen form and having an iminodiacetic acid functionality forming an ion exchange resin having said scandium absorbed thereon; Step 5 rinsing said ion exchange resin having said scandium absorbed thereon from step 4 with a dilute acid having a pH from about 1.9 to about 2.1 to remove any base metals and rare earth metals absorbed on said ion exchange resin without removing said scandium absorbed thereon; Step 6 eluting said scandium absorbed on said ion exchange resin with a solution comprising a chelating agent to form an elution solution comprising said scandium and said chelating agent; Step 7 removing said scandium from said elution solution comprising said scandium and said chelating agent by contacting said elution solution comprising said scandium and said chelating agent with a strong cation ion exchange resin being in a hydrogen form to form a strong cation ion exchange resin having said scandium absorbed thereon; Step 8 eluting said scandium absorbed on said strong cation exchange resin from step 7 with a strong acid to form a second acid solution comprising said scandium; Step 9 precipitating said scandium from said second acid solution comprising said scandium by adding a precipitating agent to said second acid solution comprising said scandium to form a scandium precipitate in a second acid solution; and Step 10 separating said scandium precipitate from said strong acid solution.
Claim 21
Dependent Claim
23 words
A method in accordance with claim 17 wherein said acid solution comprising a reducing agent in step 1 comprises hydrazine in sulfuric acid.
Claim 22
Dependent Claim
35 words
A method in accordance with claim 17 wherein said trivalent iron free acid solution comprising said scandium, divalent iron, and divalent manganese in step 2 has a pH range from about 1.5 to about 1.7.
Claim 23
Dependent Claim
53 words
A method in accordance with claim 17 wherein said step 3 comprises adjusting said trivalent free iron acid solution comprising said scandium, divalent iron, and divalent manganese from step 2 with a base to a pH of about 2.0 to form a pH adjusted solution comprising said scandium, divalent iron, and divalent manganese.
Claim 24
Dependent Claim
26 words
A method in accordance with claim 17 wherein said dilute acid of step 5 comprises a solution having a pH of about 1.9 to about 2.1.
Claim 25
Dependent Claim
38 words
A method in accordance with claim 17 wherein said chelating agent of said solution containing a chelating agent in step 6 is selected from the group consisting of diglycolic acid, carboxylic acid, hydroxy acid, EDTA, and combinations thereof.
Claim 26
Dependent Claim
24 words
A method in accordance with claim 17 wherein said chelating agent of said solution containing a chelating agent in step 6 is diglycolic acid.
Claim 27
Dependent Claim
17 words
A method in accordance with claim 17 wherein said strong acid in step 8 is 6N HCl.
Claim 28
Dependent Claim
30 words
A method in accordance with claim 17 wherein step 7 comprises precipitating said scandium from said elution solution comprising said scandium with oxalic acid to form a scandium oxalate precipitate.
References Cited (Backward Citations)
US2874039A
Cited
US3013859A
Cited
US4624703A
Cited
US4626280A
Cited
US4718995A
Cited
US4718996A
Cited
US4765909A
Cited
US4751061A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1992-03-27 | 1992-09-26 | 1993-03-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1996-03-27 | 1996-09-26 | 1997-03-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2000-03-27 | 2000-09-26 | 2001-03-28 | $7700.00 | Window Closed / Lapsed |