Gte Products Corporation

Gte Sylvania Incorporated

Martin B MacInnis

Clarence D Vanderpool

Tai K Kim

Richard A Scheithauer

Michael J Miller

Robert P McClintic

Alan D Douglas

Judith A Ladd

Martin C Vogt

Joseph E Ritsko

Kenneth T Reilly

L Rita Quatrini

Richard G Gingerich

James N Christini

John A Powers

James C Patton, Jr

Michael J Cheresnowsky

Howard L Acla

David J Port

Carl W Boyer

John E Landmesser

Thomas L Henson

Richard E Landry

Mary A Fedorchak

Donald H Ennis

John J Culkin

Edward L Bok

A method for converting cobalt to cobalt powder is disclosed which comprises heating a starting mixture of cobalt and zinc in a non-reacting atomosphere at a first temperature of below the boiling point of zinc up to about 900.degree. C. in a non-reacting atmosphere for a length of time sufficient to cause the alloying of a portion of the zinc and cobalt, with the weight ratio of zinc to cobalt being less than about 10. The temperature of the resulting partially alloyed mixture is slowly raised to a second temperature of from about 900.degree. C. to about 960.degree. and is maintained for a time sufficient only to form a reaction product in which essentially all of the cobalt is alloyed with zinc and to keep the evaporation of zinc to a minimum. The reaction product is then heated at a pressure below atmospheric pressure at a third temperature of no greater than about 950.degree. C. for a time sufficient to evaporate essentially all of the zinc and produce a cobalt ingot which is pulverizable when cooled to room temperature.

Method for converting cobalt to cobalt metal powder

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.degree. 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.

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

An improvement is disclosed in a process wherein tungsten values are extracted from an aqueous alkali metal tungstate solution by an organic extractant, and then stripped from the organic with an ammonia solution, the improvement being removing bromine from the major portion of the stripped organic and thereafter using at least a portion of the resulting bromine-free stripped organic to make up at least a portion of the organic extractant.

Process for extracting tungsten from alkali metal tungstate solutions

A process is disclosed for recovering tungsten from tungsten bearing material containing arsenic. The process involves adjusting a water slurry of the material to a pH of less than about 4 with an acid to solubilize the major portion of the tungsten, adding an insoluble ferric compound to the slurry to form a two phase system in which the solid phase contains the major portion of the arsenic and of any phosphorus which may be present, and a solution phase containing the major portion of the tungsten. After separation of the solid from the solution, the solution is adjusted to a pH of less than about 2 with an acid and a suffficient amount of hexamethylenetetramine is added to the solution to precipitate the major portion of the tungsten, followed by separating the precipitate from the resulting liquor. The solid phase containing the arsenic and phosphorus, if any, can be contacted with water and a soluble ferric salt to produce a treated solid which passes the EP toxicity test.

Process for recovering tungsten from tungsten bearing material

A method is disclosed for purifying molybdenum which involves reducing a molybdenum compound selected from the group consisting of molybdenum trioxide, ammonium dimolybdate, and ammonium paramolybdate to molybdenum dioxide which is then water washed to remove potassium, and produce a purified molybdenum dioxide having a potassium content of no greater than about 30 weight ppm, followed by separating the wash water from the purified molybdenum dioxide.

Method for purifying molybdenum

A process is disclosed for recovering scandium from a tungsten bearing material containing tungsten, iron manganese and scandium. The process involves digesting the material in an aqueous solution selected from the group consisting of a saturated solution of sulfur dioxide and a sulfuric acid solution containing an additional reducing agent at a sufficient temperature for a sufficient time to form a digestion solution containing the major portion of the scandium, iron, and manganese, and a digestion solid containing the major portion of the tungsten which is separated from the digestion solution. The major portion of the scandium is extracted from the digestion solution with an organic consisting essentially of an extracting agent which is essentially a mixture of alkyl primary amines which are present in an amount sufficient to extract the major portion of the scandium without extracting appreciable amounts of iron and manganese, and the balance an essentially aromatic solvent. After separation of the scandium containing organic from the raffinate, the organic is stripped of the scandium with hydrochloric acid which is then separated from the stripped organic. In an optional additional steps, iron is recovered by adjusting the pH of the raffinate to precipitate the major portion of the iron and manganese which is separated from the resulting liquor. A sufficient amount of chlorine gas is contacted with an aqueous slurry of the precipitate at a sufficient temperature for a sufficient time to form a manganese containing solution containing the major portion of the manganese which was in the precipitate and a solid containing the major portion of the iron which was in the precipitate.

A method is disclosed for recovering tungsten from a relatively dilute ammoniacal tungsten solution. The method involves adding hexamethylenetetramine to the tungsten solution in an amount sufficient to form a hexamethylenetetramine complex then adjusting the pH to from about 1.0 to about 2.0 with a mineral acid to form a precipitate of the complex containing at least about 99% of the tungsten, and separating the precipitate from the resulting mother liquor.

Recovery of tungsten from ammoniacal solutions

A process is disclosed for recovering tungsten, iron, and manganese from tungsten bearing material. The process involves digesting the material in a sulfur dioxide solution at a sufficient temperature for a sufficient time to form a digestion solution containing the major portion of the scandium, iron, and manganese, and a digestion solid containing the major portion of the tungsten which is separated from the digestion solution. The major portion of the scandium is extracted from the digestion solution with an organic consisting essentially of an extracting agent which is essentially a mixture of alkyl primary amines which are present in an amount sufficient to extract the major portion of the scandium without extracting appreciable amounts of iron and manganese, and the balance an essentially aromatic solvent. After separation of the scandium containing organic from the raffinate, the organic is stripped of the scandium with hydrochloric acid which is then separated from the stripped organic. The raffinate is adjusted to a pH of at least about 3.5 with a base to precipitate the major portion of the iron and manganese which is separated from the resulting liquor. A sufficient amount of chlorine gas is contacted with an aqueous slurry of the precipitate at a sufficient temperature for a sufficient time to form a manganese containing solution containing the major portion of the manganese which was in the precipitate and a solid containing the major portion of the iron which was in the precipitate.

A process is disclosed for producing ammonium paratungstate which involves adding hexamethylenetetramine to a first solution of ammonium tungstate, adjusting the pH to about 2 with an acid to form a precipitate which contains the major portion of the tungsten and the hexamethylenetetramine and separating the precipitate from the resulting mother liquor. The tungsten hexamethylenetetramine precipitate is then dissolved in aqueous ammonia to form a second ammonium tungstate solution which is then heated at from about 90.degree. C. to about 100.degree. C. to form a precipitate essentially all of which is ammonium paratungstate and a mother liquor which contains essentially all of the hexamethylenetetramine. The ammonium paratungstate precipitate is then separated from the mother liquor.

Process for producing ammonium paratungstate

A process is disclosed for recovering tungsten, scandium, iron, and manganese from tungsten bearing material. The process involves digesting the material in sufficient sulfuric acid at a sufficient temperature for a sufficient time in the presence of 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, separating the digestion solution from the digestion residue and extracting essentially all of the scandium from the solution with an organic consisting essentially of an extracting agent which is a dialkyl phosphoric acid which is present in an amount sufficient to extract essentially all of the scandium without extracting appreciable amounts of iron and manganese, and the balance an essentially aromatic solvent. The scandium containing organic is removed from the raffinate and stripped of the scandium with an aqueous ammonium carbonate solution which is separated from the stripped organic. The pH of the raffinate is adjusted to at least about 2 with a base and electrolyzed to remove the major portion of the iron as iron powder, which is separated from the resulting electrolyzed solution which contains the major portion of the manganese.

Recovery of tungsten, scandium, iron, and manganese values from tungsten

A method is disclosed for producing crystalline ammonium metatungstate from ammonium paratungstate. The method involves heating ammonium paratungstate in a multiple hearth furnace at from about 200.degree. C. to about 400.degree. C. to form a relatively uniformly heated ammonium paratungstate. A slurry of the heated ammonium paratungstate in water is then digested at from about 70.degree. C. to about 100.degree. C. for less than about 6 hours at relatively constant volume while maintaining the pH of the slurry at from about 4.2 to about 3.0 by the addition of ammonia as necessary to form a solution of ammonium metatungstate. The resulting ammonium metatungstate solution is then evaporated to a fraction of its original volume to concentrate it and any insolubles are removed. The ammonium metatungstate is then crystallized from the concentrated solution.

Method of producing crystalline ammonium metatungstate

A method is disclosed for producing crystalline ammonium metatungstate from ammonium paratungstate. The method involves heating the ammonium paratungstate at from about 100.degree. C. to about 250.degree. C. for from about 1 hour to about 8 hours to remove some ammonia and water, digesting a solution of the heated ammonium paratungstate in water at from about 80.degree. C. to about 100.degree. C. for from about 2 hours to about 6 hours at relatively constant volume while maintaining the pH of the slurry at from about 4.2 to about 3.0 by addition of ammonia as necessary to form a solution of ammonium metatungstate in water. The ammonium metatungstate solution is then evaporated to concentrate it. Any insoluble material is separated from the solution. Ammonium metatungstate is then crystallized from the resulting concentrated ammonium metatungstate solution.

A process is disclosed for recovering cobalt and chromium from a cobalt and chromium containing alloy. The process involves first digesting the alloy in concentrated hydrochloric acid at a sufficient temperature for a sufficient time to form a first solution containing the major portion of the cobalt, chromium, and any iron and nickel present in the alloy and a first solid and separating the first solution from the first solid. Oxalic acid is then added to the first solution in an amount sufficient to subsequently precipitate the major portion of the cobalt and any iron and nickel contained in the first solution followed by adjustment of the ph to from about 1 to about 2 with a base and maintaining the temperature below about 20.degree. for a sufficient time to form a second solid containing the major portion of the cobalt and the major portion of any iron and nickel which is present in the first solution and a second solution containing the major portion of the chromium which is present in the first solution and separation of the second solid from the second solution. The second solid is then washed with sufficient water to remove any water soluble impurities and separated from the resulting wash water. The resulting washed second solid is then contacted with a calcium chloride solution of sufficient calcium chloride concentration, at a sufficient temperature, for a sufficient time to form a third solution containing the major portion of the cobalt which was present in the second solid, and a third solid. The third solution is then separated from the third solid.

Recovery of cobalt and chromium

An improvement is disclosed in a process for recovery of cobalt from cobalt bearing material to obtain fine cobalt metal powder of high purity, the improvement being mechanically compacting the powder into a billet and sintering the billet in a hydrogen atmosphere at a sufficient temperature for a sufficient time to densify the billet and form a high purity cobalt article having an oxygen content of no greater than about 500 weight parts per million.

High purity cobalt article

A process is disclosed for recovering tungsten and rhenium from a tungsten and rhenium source. The process involves firing the source in an oxidizing atmosphere at a sufficient temperature for a sufficient time to convert the tungsten and rhenium to their respective oxides, to remove a portion of the rhenium as volatilized oxide, and to form a first fired material containing essentially all of the tungsten and the remaining portion of the rhenium, increasing the surface area of the resulting oxidized tungsten, and firing the first fired material in an oxidizing atmosphere at a sufficient temperature for a sufficient time to remove essentially all of the remaining portion of the rhenium as volatilized oxidized rhenium and to form an essentially rhenium-free oxidized tungsten.

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Towanda, PA, United States of America

Martin B MacInnis