# US 4,397,821 A · Precipitation of synthetic scheelite

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- Number: US 4,397,821 A
- Document ID: US4397821A
- Status: Granted
- Kind: A
- Application number: 06/337,558
- Filed: 1982-01-04
- Granted: 1983-08-09
- Earliest claimed: 1982-01-04
- Assignees: Amax Inc.
- Inventors: Leo W. Beckstead; Paul B. Queneau
- Web page: https://patentgrep.com/patent/US4397821A

## CPC

- C01G 41/00: Compounds of tungsten
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)

## Abstract

Synthetic scheelite (calcium tungstate) having a low sulfur content is produced in high yield from an aqueous solution of sodium tungstate, that can be contaminated with sulfate ion dissolved therein, by digesting the solution with solid calcium sulfate whereby low-sulfur calcium tungstate precipitates. The solution remaining after filtration of the calcium tungstate product can be treated with calcium sulfate to precipitate additional purified calcium tungstate or to generate a calcium tungstate-calcium sulfate mixture that can be recycled for digestion with additional sulfate-contaminated sodium tungstate solution.

## Claims

### Claim 1

A process for producing low-sulfur calcium tungstate from an aqueous feed solution of alkali tungstate, comprising
(a) slurrying in said solution a precipitant comprising finely divided calcium sulfate in an amount up to the stoichiometric amount based on the tungstate in the solution,
(b) digesting the slurry formed in step (a) while maintaining the pH value of the slurry between about 9 and about 12 and under conditions such that essentially all the calcium sulfate reacts with alkali tungstate, thereby forming low-sulfur calcium tungstate which is slurried in a pregnant solution containing dissolved therein alkali sulfate, and
separating the low-sulfur calcium tungstate from the pregnant solution.

### Claim 2 (depends on 1)

A process according to claim 1 wherein the pregnant solution also contains alkali tungstate dissolved therein, and further comprising subjecting the pregnant solution anew to steps (a) and (b).

### Claim 3 (depends on 1)

A continuous process for producing low-sulfur calcium tungstate from an aqueous feed solution of alkali tungstate, comprising the steps set forth in claim 1, wherein the pregnant solution formed in step (b) also contains alkali tungstate dissolved therein, and further comprising
(d) slurrying the pregnant solution recovered in step (c) with a calcium ion source in an amount which is effective to provide at least the stoichiometric requirement of calcium based on the tungstate dissolved in the pregnant solution and which is effective to provide in the slurry an amount of calcium sulfate ranging from zero up to the amount thereof required in step (a),
(e) digesting the slurry formed in step (d) under conditions such that precipitation of tungstate from the pregnant solution is maximized, thereby forming a finely divided solid product comprising calcium tungstate and calcium sulfate, slurried in an aqueous solution of alkali sulfate,
(f) filtering the finely divided solid product formed in step (e) from the aqueous solution, and
(g) recycling the finely divided solid product recovered in step (f) to step (a).

### Claim 4 (depends on 1, 2, 3)

The process of claim 1, 2 or 3 wherein the alkali tungstate in the aqueous feed solution is sodium tungstate.

### Claim 5 (depends on 1, 2, 3)

The process of claim 1, 2 or 3 wherein the aqueous feed solution is contaminated with up to about 150 gpl SO.sub.4.sup.-2.

### Claim 6 (depends on 4)

The process of claim 4 wherein the aqueous feed solution is contaminated with about 25 gpl to about 150 gpl SO.sub.4.sup.-2.

### Claim 7 (depends on 1, 2, 3)

The process of claim 1, 2 or 3 wherein the solution slurried in step (a) contains tungstate equivalent to about 5 gpl to about 300 gpl WO.sub.3.

### Claim 8 (depends on 3)

The process of claim 3 wherein the calcium ion source in step (d) comprises calcium sulfate.

### Claim 9 (depends on 1, 2, 3)

The process of claim 1, 2 or 3 wherein the low-sulfur calcium tungstate formed in step (c) contains less than about 0.5 percent S.

### Claim 10 (depends on 3)

The process of claim 3 wherein the aqueous solution of sodium sulfate formed in step (e) contains tungstate equivalent to less than about 1000 ppm WO.sub.3.

### Claim 11 (depends on 1)

The process as described in claim 1 wherein the pH value of the slurry is maintained between about 10 and about 11.