# US 2014/0193317 A1 · Methods of Recovering Scandium from Titanium Residue Streams

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- Number: US 2014/0193317 A1
- Document ID: US20140193317A1
- Status: Published application
- Kind: A1
- Application number: 14/151,177
- Filed: 2014-01-09
- Published: 2014-07-10
- Earliest claimed: 2013-01-10
- Assignees: Bloom Energy Corporation
- Applicants: Bloom Energy Corporation
- Inventors: Christopher Jeffrey Hartley; Wayne Werneke Hazen; David Ross Baughman; Christel Maria Angelina Bemelmans; Pavel Federovich Belits; Timothy James Lanyk; Brook Forest Porter; Lunzhi Liao; Justin McAllister; Michael Shang-Yu Yang
- Web page: https://patentgrep.com/patent/US20140193317A1

## CPC

- C22B 59/00: Obtaining rare earth metals
- C22B 3/26: by liquid-liquid extraction using organic compounds
- C22B 3/42: by ion-exchange extraction
- Y02P 10/20: Recycling
- C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A method for selectively removing scandium from a scandium-containing feed solution includes contacting the scandium-containing feed solution with a solvent stream in plural stages using cross current extraction, in which the solvent is loaded with at least a portion of the scandium from the feed solution, and/or ion exchange, and separating the loaded solvent from remaining scandium-containing feed solution.

## Claims

### Claim 1

A method of selectively removing scandium from a scandium-containing feed solution, comprising:
contacting the scandium-containing feed solution with a solvent stream in plural stages using cross current extraction, wherein the solvent is loaded with at least a portion of the scandium from the scandium-containing feed solution; and
separating the loaded solvent from remaining scandium-containing feed solution.

### Claim 2 (depends on 1)

The method of claim 1, wherein:
the step of contacting comprises:
contacting the scandium-containing feed solution with a barren first solvent stream in a first stage, wherein the first solvent stream is loaded with at least a portion of the scandium from the scandium-containing feed solution; and
contacting the remaining scandium-containing feed solution from the first stage with a barren second solvent stream in a second stage, wherein the second solvent stream is loaded with at least a portion of the scandium from the remaining scandium-containing feed solution from the first stage; and
the step of separating comprises:
separating the loaded first solvent from the remaining scandium-containing feed solution from the first stage; and
separating the loaded second solvent from remaining scandium-containing feed solution from the second stage.

### Claim 3 (depends on 2)

The method of claim 2, wherein:
the step of contacting further comprises contacting the remaining scandium-containing feed solution from the second stage with a barren third solvent stream in a third stage, wherein the third solvent stream is loaded with at least a portion of the scandium from the remaining scandium-containing feed solution from the second stage; and
the step of separating further comprises separating the loaded third solvent from the remaining scandium-containing feed solution from the third stage.

### Claim 4

(canceled)

### Claim 5 (depends on 3)

The method of claim 3, wherein the first, second and third stages are performed respectively in first, second, and third extraction units, and the first, second and third extraction units are connected in series to form a cross-current array.

### Claim 6 (depends on 3)

The method of claim 3, further comprising collecting the separated loaded first, second and third solvent streams in a single loaded solvent stream.

### Claim 7 (depends on 1)

The method of claim 1, wherein the solvent stream contains an extractant, wherein the extractant forms a Sc-extractant complex with scandium to load at least the portion of the scandium from the scandium-containing feed solution in the solvent stream.

### Claim 8

(canceled)

### Claim 9

(Cancelled)

### Claim 10 (depends on 1)

The method of claim 1, wherein the scandium-containing feed solution is an aqueous solution, and wherein the solvent stream is an organic liquid phase.

### Claim 11 (depends on 10)

The method of claim 10, wherein the aqueous solution is an acid solution generated as waste liquor from titanium processing.

### Claim 12

(canceled)

### Claim 13 (depends on 10)

The method of claim 10, further comprising:
scrubbing spent aqueous solution that remains after the plural stages of contacting the scandium-containing feed solution with a solvent stream; and
scrubbing the loaded organic phase with an acid solution to remove at least one of zirconium impurities and titanium impurities.

### Claim at position 14

14-19. (canceled)

### Claim 20 (depends on 10)

The method of claim 10, further comprising:
unloading scandium ions from the organic phase using a sodium hydroxide (NaOH) strip solution, wherein Sc3+ ions react with anions in the strip solution to form a scandium(III) hydroxide(Sc(OH)3) precipitate: and,
collecting spent strip solution, wherein the sodium hydroxide in the spent strip solution is recycled for use in the strip solution for unloading scandium ions from the organic phase.

### Claim 21

(canceled)

### Claim 22

(canceled)

### Claim 23 (depends on 20)

The method of claim 20, further comprising;
filtering the scandium precipitate to make a filter cake containing scandium hydroxide;
leaching scandium ions from the first filter cake, wherein the scandium ions are incorporated into an effluent aqueous filtrate: and
providing the effluent aqueous solution to at least one column, wherein the scandium ions are loaded in a stationary phase.

### Claim 24

(canceled)

### Claim 25

(canceled)

### Claim 26 (depends on 23)

The method of claim 23, further comprising:
contacting the aqueous filtrate with a second organic phase containing an extractant, wherein the second organic phase is loaded with at least a portion of the Sc3+ ions from the aqueous filtrate; and
unloading the Sc3+ ions from the second organic phase by contacting the second organic phase with a water stream, wherein at least the portion of the Sc3+ ions are dissolved in the water stream to form a second aqueous solution;
contacting the second aqueous solution with oxalic acid, wherein at least the portion of the Sc3+ ions react with oxalate ions to form a scandium oxalate precipitate;
filtering the scandium oxalate precipitate to obtain a scandium oxalate product; and
calcinating the scandium oxalate product to a scandium oxide product, wherein the scandium oxide product contains about 99.9% scandium(III) oxide (Sc2O3).

### Claim at position 22

27-29. (canceled)

### Claim 30 (depends on 23)

The method of claim 23, wherein the stationary phase comprises at least one ion exchange resin.

### Claim 31 (depends on 30)

The method of claim 30, further comprising;
eluting scandium ions from the stationary phase using a second acid solution to form an eluate. wherein the second acid solution comprises hydrochloric acid (HCl) and the eluate comprises scandium chloride;
mixing the scandium chloride with a solution containing oxalic acid, wherein scandium oxalate precipitates out of the solution;
filtering the precipitated scandium oxalate to form a scandium oxalate product; and
calcinating the scandium oxalate product to a scandium oxide product, wherein the scandium oxide product is about 95% acandium(III) oxide (Sc2O3).

### Claim at position 25

32-38. (canceled)

### Claim 39

A method of producing a scandium-containing product from a titanium- and scandium-containing acid solution stream, comprising producing at least 2.0 kg/h of the scandium-containing product comprising at least 99 wt % Sc2O3 per 125,000 L/h of the acid solution stream.

### Claim 40 (depends on 39)

The method of claim 39, comprising producing 2.0 to 2.9 kg/h of the scandium-containing product comprising 99 to 99.9 wt % Sc2O3 per 125,000 L/h of the acid solution stream.

### Claim 41

(canceled)

### Claim 42

A method of selectively removing scandium from a scandium-containing feed solution, comprising:
contacting the scandium-containing feed solution with at least one ion exchange resin, such that the at least one ion exchange resin is loaded with at least a portion of the scandium from the scandium-containing feed solution;
providing an eluent solution to the at least one ion exchange resin, wherein scandium is unloaded into an eluate stream; and
converting the unloaded scandium in the eluate stream to a solid scandium oxide product.

### Claim 43 (depends on 42)

The method of claim 42, wherein the at least one ion exchange resin is located in a plurality of columns arranged in series.

### Claim 44 (depends on 42)

The method of claim 42, wherein the eluent solution provided to the-at least one ion exchange resin comprises a solution having a pKa that is greater than or equal to −2.

### Claim at position 32

45-47. (canceled)

### Claim 48 (depends on 42)

The method of claim 42, wherein:
the at least a portion of the scandium loaded in the ion exchange resin comprises at least 80% of scandium in the scandium-containing feed solution;
the concentration of scandium in the scandium-containing feed solution is less than or equal to 40 mg/mL: and
the concentration of scandium in the eluate stream is greater than 800 mg/mL.

### Claim 49

(canceled)

### Claim 50 (depends on 42)

The method of claim 42, wherein the at least one ion exchange resin comprises an ion exchange material having at least one of:
sulfur-based ligands or chelating functional groups; and
phosphorous-based ligands or chelating functional groups.

### Claim 51 (depends on 42)

The method of claim 42, further comprising refining the solid scandium oxide product such that the solid scandium oxide product comprises at least 99% scandium oxide.