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Recovery of tungsten, scandium, iron, and manganese from tungsten bearing material

Assignee: Osram Sylvania Inc
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Filing: 1987-12-21
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Granted: 1989-02-28
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Expires: 2007-12-21
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Abstract

Abstract A process is disclosed for recovering tungsten, iron, and manganese from tungsten bearing material. The process involves digesting the material in a sufficient amount of sulfuric acid at a temperature of at least about 80° C. for a sufficient time in the presence of coal as a reducing agent to form a digestion solution containing the major portion of the scandium, iron, and manganese and a digestion residue containing the major portion of the tungsten, followed by separating the solution from the residue. The major portion of the scandium can be extracted from the digestion solution with an organic solution consisting essentially of a mixture of tertiary alkyl primary amines which are present in an amount sufficient to extract the major portion of the scandium, and the balance an essentially aromatic solvent. The scandium is stripped from the organic with hydrochloric acid which is then separated from the stripped organic. The extraction can be accomplished by an organic solution consisting essentially of an extracting agent which is a dialkyl phosphoric acid and an essentially aromatic solvent. In this latter case, the stripping agent for the scandium is an aqueous solution of ammonium carbonate.

Inventors

  • 👤 Clarence D. Vanderpool
  • 👤 Judith A. Ladd
  • 👤 Martin B. MacInnis
  • 👤 Mary A. Fedorchak

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 05:40
CPC Classifications
C; C22; C22B; C22B34/00; C22B34/30; C22B34/36; C01; C01F; C01F17/00; C01F17/10; C01F17/17; C22B3/00; C22B3/04; C22B3/06; C22B3/08; C22B3/20; C22B3/26; C22B3/28; C22B3/282; C22B3/38; C22B3/384; C22B3/3846; C22B47/00; C22B59/00; Y; Y02; Y02P; Y02P10/00; Y02P10/20

Claims Analysis

Total Claims: 23
Claim 1
Independent Claim 83 words
A process for separating tungsten, from scandium, iron, and manganese in tungsten bearing material, said process comprising: (a) digesting said material in sufficient sulfuric acid at a temperature of at least about 80° C. for a sufficient time in the presence of coal as a reducing agent to form a digestion solution containing the major portion of the scandium, iron and manganese and a digestion residue containing the major portion of the tungsten; and (b) separating said digestion solution from said digestion residue.
Claim 2
Dependent Claim 83 words
A process for separating tungsten, from scandium, iron, and manganese in tungsten bearing material, said process comprising: (a) digesting said material in sufficient sulfuric acid at a temperature of at least about 80° C. for a sufficient time in the presence of coal as a reducing agent to form a digestion solution containing the major portion of the scandium, iron and manganese and a digestion residue containing the major portion of the tungsten; and (b) separating said digestion solution from said digestion residue.
Claim 3
Dependent Claim 21 words
A process of claim 1 wherein the concentration of said sulfuric acid is from about 18 normal to about 36 normal.
Claim 4
Dependent Claim 23 words
A process of claim 1 wherein said coal is present in a weight ratio of coal to manganese of about 2 to 9.
Claim 5
Dependent Claim 32 words
A process of claim 1 wherein the digestion step is carried out at a temperature of from about 80° C. to about 150° C. for from about 4 hours to 7 hours.
Claim 6
Dependent Claim 33 words
A process of claim 4 wherein said digestion step is carried out at a temperature of from about 100° C. to about 140° C. for from about 5 hours to about 7 hours.
Claim 7
Dependent Claim 190 words
A process for recovering tungsten, scandium, iron, and manganese from tungsten bearing material, said process comprising: (a) digesting said material in sufficient sulfuric acid at a temperature of at least about 80° C. for a sufficient time in the presence of coal as a reducing agent to form a digestion solution containing the major portion of the scandium, iron and manganese and a digestion residue containing the major portion of the tungsten; (b) separating said digestion solution from said digestion residue; (c) extracting the major portion of the scandium from said digestion solution with an organic solution consisting essentially of an extracting agent which is essentially a mixture of tertiary alkyl primary amines which are present in an amount sufficient to extract the major portion of the scandium, and the balance an essentially aromatic solvent; (d) separating the resulting scandium containing organic from the resulting raffinate; (e) stripping essentially all of the scandium from the scandium-containing organic solution by contacting said scandium-containing organic solution with hydrochloric acid to form a scandium containing hydrochloric acid solution; and (f) separating said scandium containing hydrochloric acid solution from the resulting stripped organic solution.
Claim 8
Dependent Claim 190 words
A process for recovering tungsten, scandium, iron, and manganese from tungsten bearing material, said process comprising: (a) digesting said material in sufficient sulfuric acid at a temperature of at least about 80° C. for a sufficient time in the presence of coal as a reducing agent to form a digestion solution containing the major portion of the scandium, iron and manganese and a digestion residue containing the major portion of the tungsten; (b) separating said digestion solution from said digestion residue; (c) extracting the major portion of the scandium from said digestion solution with an organic solution consisting essentially of an extracting agent which is essentially a mixture of tertiary alkyl primary amines which are present in an amount sufficient to extract the major portion of the scandium, and the balance an essentially aromatic solvent; (d) separating the resulting scandium containing organic from the resulting raffinate; (e) stripping essentially all of the scandium from the scandium-containing organic solution by contacting said scandium-containing organic solution with hydrochloric acid to form a scandium containing hydrochloric acid solution; and (f) separating said scandium containing hydrochloric acid solution from the resulting stripped organic solution.
Claim 9
Dependent Claim 19 words
A process of claim 6 wherein the sulfuric acid concentration is from about 18 normal to about 36 normal.
Claim 10
Dependent Claim 23 words
A process of claim 6 wherein said coal is present in a weight ratio of coal to manganese of about 2 to 9.
Claim 11
Dependent Claim 32 words
A process of claim 6 wherein the digestion step is carried out at a temperature of from about 80° C. to about 150° C. for from about 4 hours to 7 hours.
Claim 12
Dependent Claim 33 words
A process of claim 9 wherein said digestion step is carried out at a temperature of from about 100° C. to about 140° C. for from about 5 hours to about 7 hours.
Claim 13
Dependent Claim 31 words
A process of claim 6 wherein said extracting agent is essentially a mixture of tertiary alkyl primary amines wherein the alkyl groups have from about 18 to about 22 carbon atoms.
Claim 14
Dependent Claim 48 words
A process of claim 11 wherein said essentially aromatic solvent consists essentially of a mixture of alkyl benzenes wherein the alkyl benzenes have molecular weights of 120, 134, or 148, and the total number of carbon atoms attached to the benzene ring are either 3, 4, or 5.
Claim 15
Dependent Claim 19 words
A process of claim 6 wherein the hydrochloric acid concentration is from about 1 normal to about 4 normal.
Claim 16
Dependent Claim 117 words
In the process for recovering tungsten, scandium, iron and manganese from tungsten bearing materials wherein said process comprises digesting the material in sulfuric acid to form a digestion solution containing major portions scandium, iron and manganese and a digestion residue containing the major portion of the tungsten wherein the said digestion solution is separated from the digestion residue and a major portion of scandium is extracted from the digestion solution with an organic extracting agent in the presence of a aromatic solvent and the scandium is stripped from the scandium containing organic with a suitable stripping agent and thereafter separated from the strip organic, the improvement comprising utilizing coal as a reducing agent in the digestion step.
Claim 17
Dependent Claim 117 words
In the process for recovering tungsten, scandium, iron and manganese from tungsten bearing materials wherein said process comprises digesting the material in sulfuric acid to form a digestion solution containing major portions scandium, iron and manganese and a digestion residue containing the major portion of the tungsten wherein the said digestion solution is separated from the digestion residue and a major portion of scandium is extracted from the digestion solution with an organic extracting agent in the presence of a aromatic solvent and the scandium is stripped from the scandium containing organic with a suitable stripping agent and thereafter separated from the strip organic, the improvement comprising utilizing coal as a reducing agent in the digestion step.
Claim 18
Dependent Claim 19 words
A process of claim 14 wherein the sulfuric acid concentration is from about 18 normal to about 36 normal.
Claim 19
Dependent Claim 23 words
A process of claim 14 wherein said coal is present in a weight ratio of coal to manganese of about 2 to 9.
Claim 20
Dependent Claim 32 words
A process of claim 14 wherein the digestion step is carried out at a temperature of from about 80° C. to about 150° C. for from about 4 hours to 7 hours.
Claim 21
Dependent Claim 33 words
A process of claim 17 wherein said digestion step is carried out at a temperature of from about 100° C. to about 140° C. for from about 5 hours to about 7 hours.
Claim 22
Dependent Claim 13 words
A process of claim 14 wherein the extracting agent is di(2-ethylhexyl) phosphoric acid.
Claim 23
Dependent Claim 48 words
A process of claim 19 wherein said essentially aromatic solvent consists essentially of a mixture of alkyl benzenes wherein the alkyl benzenes have molecular weights of 120, 134, or 148, and the total number of carbon atoms attached to the benzene ring are either 3, 4, or 5.

References Cited (Backward Citations)

GB374250A Cited
US4028463A Cited
US4624703A Cited
US4626280A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-02-28 1992-08-29 1993-02-28 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-02-28 1996-08-29 1997-02-28 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-02-28 2000-08-29 2001-02-28 $7700.00 Window Closed / Lapsed

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