# US 8,771,617 B2 · Method for extracting tungsten from scheelite

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- Number: US 8,771,617 B2
- Document ID: US8771617B2
- Status: Granted
- Kind: B2
- Application number: 13/794,844
- Filed: 2013-03-12
- Published: 2013-08-01
- Granted: 2014-07-08
- Earliest claimed: 2010-12-24
- Assignees: Central South University
- Applicants: Central South University
- Inventors: Zhongwei Zhao; Jiangtao Li
- Web page: https://patentgrep.com/patent/US8771617B2

## CPC

- C22B 34/36: Obtaining tungsten
- C22B 3/06: in inorganic acid solutions {, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions}
- C22B 3/08: Sulfuric acid {, other sulfurated acids or salts thereof}
- 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 extracting tungsten from scheelite by: 1) adding a mixed acid including H2SO4 and H3PO4 to a decomposition reactor; 2) heating the mixed acid to a temperature of 70-100° C.; adding scheelite while controlling the mixed acid present in an amount of 3-8 L per kg of scheelite; allowing the components in the decomposition reactor to react for 1-6 h, and filtering the resulting mixture to obtain a filtrate; 3) supplementing the filtrate with sulfuric acid consumed in the reaction; 4) crystallizing the filtrate to obtain phosphotungstic acid crystals and mother liquor; 5) dissolving the phosphotungstic acid crystals in water to obtain a phosphotungstic acid solution; 6) transforming the phosphotungstic acid solution into an ammonium tungstate solution for the purpose of preparing ammonium paratungstate; and 7) supplementing the mother liquor with phosphoric acid and water to an initial level and reusing the mother liquor for ore leaching.

## Claims

### Claim 1

A method for extracting tungsten from scheelite, the method comprising the steps of:
1) adding a mixed acid comprising sulfuric acid and phosphoric acid into a decomposition reactor, wherein the sulfuric acid is present in the mixed acid at a concentration of 150-500 g/L and the phosphoric acid is present in the mixed acid at a concentration corresponding to 15-35 wt. % of P2O5;
2) heating the mixed acid to a temperature of 70-100° C.; adding scheelite to the decomposition reactor and controlling an amount of the mixed acid present in the decomposition reactor at 3-8 L per kg of scheelite; allowing components in the decomposition reactor to react for 1-6 hr, and filtering to obtain a filtrate;
3) supplementing the filtrate with sulfuric acid;
4) crystallizing the filtrate of step 3) to obtain phosphotungstic acid crystals and a mother liquor;
5) dissolving the phosphotungstic acid crystals in water to obtain a phosphotungstic acid solution;
6) transforming the phosphotungstic acid solution to an ammonium tungstate solution for preparing ammonium paratungstate (APT); and
7) supplementing the mother liquor of step 4) with phosphoric acid and water to obtain a diluted mother liquor comprising sulfuric acid and phosphoric acid at the same concentrations as those in step 1), and using the diluted mother liquor as the mixed acid in step 1) for leaching scheelite.

### Claim 2 (depends on 1)

The method of claim 1, wherein the scheelite comprises 10-75 wt. % of WO3 and has a grain size≦150 μm.

### Claim 3 (depends on 1)

The method of claim 1, wherein
the phosphotungstic acid crystals are obtained by cooling the filtrate of step 3) to 30-50° C. and filtering; or
the phosphotungstic acid crystals are obtained by concentrating the filtrate of step 3) to have a ⅓-⅘ original volume, and filtering.

### Claim 4 (depends on 1)

The method of claim 1, wherein
the phosphotungstic acid solution obtained from dissolving the phosphotungstic acid crystals comprises 350-500 g/L of WO3; and
the phosphotungstic acid solution is transformed into the ammonium tungstate solution comprising 200-300 g/L of WO3 by adding ammonia, ion exchange, or solvent extraction.

### Claim 5 (depends on 3)

The method of claim 3, wherein
the phosphotungstic acid solution obtained from dissolving the phosphotungstic acid crystals comprises 350-500 g/L of WO3; and
the phosphotungstic acid solution is transformed into the ammonium tungstate solution comprising 200-300 g/L of WO3 by adding ammonia, ion exchange, or solvent extraction.

### Claim 6

A method for extracting tungsten from scheelite, the method comprising:
1) adding a mixed acid comprising sulfuric acid and phosphoric acid into a decomposition reactor, wherein the sulfuric acid is present in the mixed acid at a concentration of 150-500 g/L and the phosphoric acid is present in the mixed acid at a concentration corresponding to 15-35 wt. % of P2O5;
2) heating the mixed acid to a temperature of 70-100° C.; adding scheelite to the decomposition reactor, leaching scheelite in the mixed acid, and controlling an amount of the mixed acid present in the decomposition reactor at 3-8 L per kg of scheelite; allowing components in the decomposition reactor to react for 1-6 hr, and filtering to obtain a filtrate;
3) supplementing the filtrate with sulfuric acid;
4) crystallizing the filtrate of step 3) to obtain phosphotungstic acid crystals and a mother liquor;
5) dissolving the phosphotungstic acid crystals in water to obtain a phosphotungstic acid solution; and
6) transforming the phosphotungstic acid solution to an ammonium tungstate solution for preparing ammonium paratungstate.

### Claim 7 (depends on 6)

The method of claim 6, wherein the method further comprises supplementing the mother liquor of step 4) with phosphoric acid and water to obtain a diluted mother liquor comprising sulfuric acid and phosphoric acid at the same concentrations as those in step 1), using the diluted mother liquor as the mixed acid in step 1) for leaching scheelite, and repeating steps 2)-6).

### Claim 8 (depends on 6)

The method of claim 6, wherein the scheelite comprises 10-75 wt. % of WO3 and has a grain size≦150 μm.

### Claim 9 (depends on 6)

The method of claim 6, wherein
the phosphotungstic acid crystals are obtained by cooling the filtrate of step 3) to 30-50° C. and filtering; or
the phosphotungstic acid crystals are obtained by concentrating the filtrate of step 3) to have a ⅓-⅘ original volume, and filtering.

### Claim 10 (depends on 6)

The method of claim 6, wherein
the phosphotungstic acid solution obtained from dissolving the phosphotungstic acid crystals comprises 350-500 g/L of WO3; and
the phosphotungstic acid solution is transformed into the ammonium tungstate solution comprising 200-300 g/L of WO3 by adding ammonia, ion exchange, or solvent extraction.

### Claim 11 (depends on 9)

The method of claim 9, wherein
the phosphotungstic acid solution obtained from dissolving the phosphotungstic acid crystals comprises 350-500 g/L of WO3; and
the phosphotungstic acid solution is transformed into the ammonium tungstate solution comprising 200-300 g/L of WO3 by adding ammonia, ion exchange, or solvent extraction.