Process of purifying and separating columbium and tantalum values from each other

Claim 1

A METHOD FOR PRODUCING SEPARATE SOLUTIONS OF COLUMBIUM AND TANTALUM VALUES FROM A STARTING MIXTURE CONTAINING SAID VALVES AND ALSO CONTAINING AS IMPURITIES A COMPOUND OF A METAL SELECTED FROM THE GROUP CONSISTING OF TITANIUM, IRON, SILICON, ALUMINUM, ZIRCONIUM, TIN, MANGANESE, CALCIUM, SODIUM, TUNGSTEN, MOLYBDENUM, POTASSIUM, MAGNESIUM, BARIUM AND STRONTIUM, WHICH METALS FORM A COMPOUND SELECTED FROM THE GROUP CONSISTING OF FLUORIDES AND FLUO-ACIDS WHICH COMPOUND IS SOLUBLE IN WATER AND IS LESS SOLUBLE THAN ARE FLUOCOLUMBIC AND FLUOTANTALIC ACIDS IN A SUBSTANTIALLY WATER-IMMISCIBLE ORGANIC SOLVENT SELECTED FROM THE GROUP CONSISTING OF METHYL ISOBUTYL KETONE, DIETHYL KETONE, CYCLOHEXONE, DIISOBUTYL KETONE, TRIBUTYL, PHOSPHATE, AND MUTUALLY SOLUBLE MIXTURES THEREOF, WHICH COMPRISES: FORMING FORM SAID STARTING MIXTURE A SOLUTION OF FLUOCOLUMBIC ACID AND FLUOTANTALIC ACID IN A SOLVENT SELECTED FROM THE GROUP CONSISTING OF WATER AND SAID ORGANIC SOLVENTS, SAID SOLUTION WHEN FORMED IN AN ORGANIC SOLVENT HAVING A HYDROGEN ION CONCENTRATION OF AT LEAST ABOUT 8 NORMAL AND WHEN AN AQUEOUS SOLUTION OF AT LEAST ABOUT 13 NORMAL, SAID SOLUTION ALSO CONTAINING A COMPOUND SELECTED FROM THE GROUP CONSISTING OF A FLUORIDE AND A FLUO-ACID OF ONE OF SAID METAL IMPURITIES PRESENT IN SAID STARTING MATERIAL; INTRODUCING SAID SOLUTION INTO AN INTERMEDIATE STAGE OF A MULTI-STAGE COUNTERCURRENT EXTRACTION SYSTEM EMPLOYING TWO SOLVENTS, ONE SOLVENT BEING SELECTED FROM THE GROUP OF SUBSTANTIALLY WATERIMMISCIBLE ORGANIC SOLVENTS AND THE OTHER BEING AN ACIDIC AQUEOUS SOLVENT HAVING A HYDROGEN ION CONCENTRATION OF ABOUT 10 NORMAL TO ABOUT 18 NORMAL, TO PREFERENTIALLY EXTRACT FLUORIDES AND FLUO-ACIDS OF SAID METAL IMPURITIES TO THE AQUEOUS PHASE OF SAID EXTRACTION SYSTEM AND FLUOCOLUMBIC AND FLUOTANTALIC ACIDS TO THE ORGANIC PHASE OF SAID EXTRACTION SYSTEM; INTRODUCING SAID ORGANIC PHASE CONTAINING SAID FLUOCOLUMBIC AND FLUOTANTALIC ACIDS INTO AN INTERMEDIATE STAGE OF A SECOND MULTI-STAGE COUNTERCURRENT EXTRACTION SYSTEM EMPLOYING TWO SOLVENTS, ONE SOLVENT BEING SELECTED FROM SAID GROUP OF SUBSTANTIALLY WATER-IMMISCIBLE ORGANIC SOLVENTS AND THE OTHER BEING AN ACIDIC AQEUOUS SOLVENT HAVING A HYDROGEN ION CONCENTRATION OF ABOUT 0.5 NORMAL TO ABOUT 4 NORMAL, WHEREBY THE MIXING OF SAID AQUEOUS SOLVENT AND SAID FEED SOLUTION PRODUCES A HYDROGEN ION CONCENTRATION AT WHICH AT LEAST PART OF THE FLUOCOLUMBIC ACID OF SAID ORGANIC PHASE IS CONVERTED TO A MORE WATER SOLUBLE FLUORINE COMPOUND OF COLUMBIUM, TO PREFERENTIALLY EXTRACT SAID FLUORINE COMPOUND OF COLUMBIUM TO THE AQEUOUS PHASE OF SAID SECOND EXTRACTION SYSTEM AND FLUOTANTALIC ACID TO THE ORGANIC PHASE OF SAID SECOND EXTRACTION SYSTEM, THE ORGANIC SOLVENTS EMPLOYED IN SAID TWO EXTRACTION SYSTEMS BEING MUTUALLY SOLUBLE; AND BRINGING SAID LAST MENTIONED ORGANIC PHASE CONTAINING FLUOTANTALIC ACID INTO CONTACT WITH A SCRUB LIQUID SELECTED FROM THE GROUP CONSISTING OF WATER AND A DILUTE AQUEOUS SOLUTION OF A MINERAL ACID SELECTED FROM THE GROUP CONSISTING OF SULFURIC ACID, NITRIC ACID, HYDROFLUORIC ACID, HYDROCHLORIC ACID, PERCHLORIC ACID, PHOSPHORIC ACID AND COMPATABLE MIXTURES OF SAID ACIDS TO PREFERENTIALLY EXTRACT SAID FLUOTANTALIC ACID TO THE RESULTING AQUEOUS PHASE.

Claim 2

A METHOD FOR PRODUCING SEPARATE SOLUTIONS OF COLUMBIUM AND TANTALUM VALUES FROM A STARTING MIXTURE CONTAINING SAID VALVES AND ALSO CONTAINING AS IMPURITIES A COMPOUND OF A METAL SELECTED FROM THE GROUP CONSISTING OF TITANIUM, IRON, SILICON, ALUMINUM, ZIRCONIUM, TIN, MANGANESE, CALCIUM, SODIUM, TUNGSTEN, MOLYBDENUM, POTASSIUM, MAGNESIUM, BARIUM AND STRONTIUM, WHICH METALS FORM A COMPOUND SELECTED FROM THE GROUP CONSISTING OF FLUORIDES AND FLUO-ACIDS WHICH COMPOUND IS SOLUBLE IN WATER AND IS LESS SOLUBLE THAN ARE FLUOCOLUMBIC AND FLUOTANTALIC ACIDS IN A SUBSTANTIALLY WATER-IMMISCIBLE ORGANIC SOLVENT SELECTED FROM THE GROUP CONSISTING OF METHYL ISOBUTYL KETONE, DIETHYL KETONE, CYCLOHEXONE, DIISOBUTYL KETONE, TRIBUTYL, PHOSPHATE, AND MUTUALLY SOLUBLE MIXTURES THEREOF, WHICH COMPRISES: FORMING FORM SAID STARTING MIXTURE A SOLUTION OF FLUOCOLUMBIC ACID AND FLUOTANTALIC ACID IN A SOLVENT SELECTED FROM THE GROUP CONSISTING OF WATER AND SAID ORGANIC SOLVENTS, SAID SOLUTION WHEN FORMED IN AN ORGANIC SOLVENT HAVING A HYDROGEN ION CONCENTRATION OF AT LEAST ABOUT 8 NORMAL AND WHEN AN AQUEOUS SOLUTION OF AT LEAST ABOUT 13 NORMAL, SAID SOLUTION ALSO CONTAINING A COMPOUND SELECTED FROM THE GROUP CONSISTING OF A FLUORIDE AND A FLUO-ACID OF ONE OF SAID METAL IMPURITIES PRESENT IN SAID STARTING MATERIAL; INTRODUCING SAID SOLUTION INTO AN INTERMEDIATE STAGE OF A MULTI-STAGE COUNTERCURRENT EXTRACTION SYSTEM EMPLOYING TWO SOLVENTS, ONE SOLVENT BEING SELECTED FROM THE GROUP OF SUBSTANTIALLY WATERIMMISCIBLE ORGANIC SOLVENTS AND THE OTHER BEING AN ACIDIC AQUEOUS SOLVENT HAVING A HYDROGEN ION CONCENTRATION OF ABOUT 10 NORMAL TO ABOUT 18 NORMAL, TO PREFERENTIALLY EXTRACT FLUORIDES AND FLUO-ACIDS OF SAID METAL IMPURITIES TO THE AQUEOUS PHASE OF SAID EXTRACTION SYSTEM AND FLUOCOLUMBIC AND FLUOTANTALIC ACIDS TO THE ORGANIC PHASE OF SAID EXTRACTION SYSTEM; INTRODUCING SAID ORGANIC PHASE CONTAINING SAID FLUOCOLUMBIC AND FLUOTANTALIC ACIDS INTO AN INTERMEDIATE STAGE OF A SECOND MULTI-STAGE COUNTERCURRENT EXTRACTION SYSTEM EMPLOYING TWO SOLVENTS, ONE SOLVENT BEING SELECTED FROM SAID GROUP OF SUBSTANTIALLY WATER-IMMISCIBLE ORGANIC SOLVENTS AND THE OTHER BEING AN ACIDIC AQEUOUS SOLVENT HAVING A HYDROGEN ION CONCENTRATION OF ABOUT 0.5 NORMAL TO ABOUT 4 NORMAL, WHEREBY THE MIXING OF SAID AQUEOUS SOLVENT AND SAID FEED SOLUTION PRODUCES A HYDROGEN ION CONCENTRATION AT WHICH AT LEAST PART OF THE FLUOCOLUMBIC ACID OF SAID ORGANIC PHASE IS CONVERTED TO A MORE WATER SOLUBLE FLUORINE COMPOUND OF COLUMBIUM, TO PREFERENTIALLY EXTRACT SAID FLUORINE COMPOUND OF COLUMBIUM TO THE AQEUOUS PHASE OF SAID SECOND EXTRACTION SYSTEM AND FLUOTANTALIC ACID TO THE ORGANIC PHASE OF SAID SECOND EXTRACTION SYSTEM, THE ORGANIC SOLVENTS EMPLOYED IN SAID TWO EXTRACTION SYSTEMS BEING MUTUALLY SOLUBLE; AND BRINGING SAID LAST MENTIONED ORGANIC PHASE CONTAINING FLUOTANTALIC ACID INTO CONTACT WITH A SCRUB LIQUID SELECTED FROM THE GROUP CONSISTING OF WATER AND A DILUTE AQUEOUS SOLUTION OF A MINERAL ACID SELECTED FROM THE GROUP CONSISTING OF SULFURIC ACID, NITRIC ACID, HYDROFLUORIC ACID, HYDROCHLORIC ACID, PERCHLORIC ACID, PHOSPHORIC ACID AND COMPATABLE MIXTURES OF SAID ACIDS TO PREFERENTIALLY EXTRACT SAID FLUOTANTALIC ACID TO THE RESULTING AQUEOUS PHASE.