Abstract: A method of selectively removing impurities from a scandium-containing feed solution includes contacting an aqueous scandium-containing solution with an organic solvent stream containing an extractant, thereby forming a loaded organic solvent stream containing the impurity or impurities while leaving the scandium in the raffinate. The aqueous stream containing the scandium is washed, diluted and has inorganic salts added before being contacted with a second organic solvent stream to extract the scandium selectively, and followed by stripping the scandium from the scandium-containing loaded organic extractant stream by adding oxalic acid to the loaded organic extractant stream to form scandium oxalate.

Abstract: The present invention provides for a composition comprising an inorganic scintillator comprising an alkali metal hafnate, optionally cerium-doped, having the formula A2HfO3:Ce; wherein A is an alkali metal having a valence of 1, such as Li or Na; and the molar percent of cerium is 0% to 100%. The alkali metal hafnate are scintillators and produce a bright luminescence upon irradiation by a suitable radiation.

Abstract: A separation method of zirconium and hafnium is described which includes an extraction process of agitating an undiluted aqueous solution containing zirconium, hafnium, and sulfuric acid with a first stirring solution containing an acidic extractant to produce a first extract solution in which the hafnium is extracted by the acidic extractant; and a recovery process of agitating the first extract solution with a second stirring solution containing a citric acid solution to produce a citric acid solution after extraction in which zirconium is reverse-extracted from the first extract solution to the citric acid solution so as to recover zirconium contained in the first extract solution. The method may reduce the amount of extractant while greatly enhancing the separation effect of zirconium and hafnium, and increase zirconium recovery rate by more than 97% through an additional zirconium recovery process while reducing a hafnium content in zirconium by less than 50 ppm.

Abstract: A process for leaching a value metal from a titanium-bearing ore material comprising the step of leaching the ore material at atmospheric pressure with a lixiviant comprising a chloride and hydrochloric acid is disclosed. The leaching conditions are such that titanium is leached and remains in solution. The temperature is maintained at less that 85° C., and the concentration of hydrochloric acid is preferably less than 20% (mass ratio). The preferred chloride is magnesium chloride. The lixiviant may contain oxidant e.g. sodium chlorate or chlorine.

Abstract: A process for the separation and purification of hafnium and zirconium.

Abstract: A method of manufacturing high purity hafnium is provided and includes the steps of making aqueous solution of chloride of hafnium, thereafter removing zirconium therefrom via solvent extraction, performing neutralization treatment to obtain hafnium oxide, further performing chlorination to obtain hafnium chloride, obtaining hafnium sponge via reducing said hafnium chloride, and performing electron beam melting to the hafnium sponge in order to obtain a hafnium ingot, as well as a high purity hafnium material obtained thereby and a target and thin film formed from such material. The present invention relates to a high purity hafnium material with reduced zirconium content contained in the hafnium, a target and thin film formed from such material, and the manufacturing method thereof, and provides efficient and stable manufacturing technology, a high purity hafnium material obtained according to such manufacturing technology, and a target and high purity hafnium thin film formed from such material.

Abstract: A method of separating zirconium and hafnium tetrachlorides using a solvent comprising firstly an alkaline metallic solvent comprising a salt made up of an alkali metal chloride and an acidic metal chloride A, for example a chloroaluminate or an alkaline chloroferrate, and secondly an acidic metal or metalloid chloride B of acidity that is less than that of the acidic metal chloride A. The acidic metal or metalloid chloride B may be selected from chlorides of Mg, Zn, and Cu. The method may be a continuous separation method by selective absorption of the tetrachloride vapors by the solvent in the substantially or totally molten state.

Abstract: A method is provided to optimize separation of zirconium from hafnium by extraction of a feed mix including (Zr+Hf)OCl2 with a thiocyanate-containing organic phase. The method includes maintaining the TA/MO2 ratio in a range from greater than about 2.55 to about 3.5.

Abstract: A method and system for improved ion exchange chromatographic elemental separations of zirconium and hafnium elements and also, if desired, separations of the isotopes thereof from crude zirconium minerals by using improved crude aqueous zirconium (also containing hafnium) chloride feedstock solutions, aqueous chloride eluant solutions, cationic or anionic exchange resins, and reduced ion exchange chromatographic operating temperatures. The method and system of the invention provides improved crude aqueous zirconium chloride feedstock solutions by carbochlorinating zircon sand and hydrolyzing and dissolving the chlorination products under controlled conditions to substantially eliminate cross-polymerization of the carbochlorination products, which undesirably yield inseparable zirconium and hafnium co-polymers during hydrolysis, by inhibiting the hydrolysis exotherm and/or the free acid generation during hydrolysis.

Abstract: A method and system for improved continuous ion exchange chromatographic elemental separations of zirconium and hafnium and also for isotopic separations thereof from crude zirconium minerals by using zirconium (also containing hafnium) sulfate feedstock solutions, sulfate eluant solutions, anionic exchange resins, and reduced ion exchange column operating temperatures. The method and system of the invention provides sulfate feedstock solutions by completely converting the carbochlorination products of zircon sand to sulfate solutions prior to feeding to the ion exchange chromatographic column. The method and system of the invention is performed in a continuously operating continuous annular chromatograph (CAC). Nuclear grade substantially purified zirconium and hafnium metals are produced.

Abstract: Zirconium tetrachloride containing hafnium tetrachloride is selectively reduced with liquid metallic tin to produce zirconium trichloride. The hafnium tetrachloride is then separated as a vapor from a slurry of zirconium trichloride and other solids, including stannous dichloride, in liquid metallic tin.

Abstract: A process for separating zirconium values from hafnium values wherein an aqueous solution of ZrCl.sub.4 and HfCl.sub.4 is contacted with NH.sub.4 SCN, feeding the resultant solution into a solvent extraction system containing aqueous HCl and MIBK, separating off the solvent phase containing MIBK, HSCN, hafnium thiocyanate complex, and any decomposition products of HSCN to leave the aqueous phase raffinate containing NH.sub.4 Cl, zirconium oxide-chloride and low concentrations of HSCN, scrubbing the hafnium values from the separated solvent phase, treating the scrubbed solvent phase containing MIBK and HSCN with NH.sub.4 OH to convert the HSCN to NH.sub.4 SCN, separating the NH.sub.4 SCN from the treated solvent phase, treating the separated solvent phase to remove essentially all thiazolines, and scrubbing residual HSCN from the raffinate with the desulfurized solvent phase.

Abstract: The thermal neutron capture cross-section of zirconium may be altered by altering its natural isotope distribution through a steady state chromatographic separation of these isotopes using an anion exchange resin as the stationary phase of the chromatographic column. Zirconium is dissolved in a very strong acid which causes the formation of a zirconium anion, such as the ZrOCl.sub.4.sup.-2 anion formed in six normal hydrochloric acid, and eluted off the column with a weaker acid. Distinct elution volumes representative of each isotope are collected. In a preferred embodiment, the process also separates the zirconium from hafnium and the other impurities normally present in the product obtained by chlorinating zircon sand and utilizes a continuous annular chromatograph.

Abstract: A simple, low cost continuous process for separating and purifying zirconium and hafnium which eliminates liquid waste and facilitates the management of RCRA and LLW wastes is provided. An aqueous zirconium and hafnium--containing feed solution is prepared and fed to a continuously rotating annular chromatograph containing a bed of acid exchange resin. An acid eluant, such as hydrochloric acid, nitric acid, phosphoric acid or the like, is fed through the acid exchange bed while chromatograph is rotating, which separates the feed into substantially pure zirconium and hafnium fractions and into RCRA and LLW waste fractions. The zirconium and hafnium are processed further into nuclear quality zirconium and hafnium metals. The acid eluant is recycled for reuse in the chromatograph, and the RCRA and LLW waste fractions are disposed of in solid form.

Abstract: The isotopes of zirconium can be partially or completely separated by loading an aqueous solution of an ionic compound of zirconium onto a cationic exchange resin with pentavalent phosphorus derived active groups which serves as the stationary phase of a chromatograph, eluting the compound with an aqueous acid and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the eluant is a strong mineral acid, such as hydrochloric acid and the chromatograph is of a type, such as a continuous annular chromatograph, that it can be operated in a continuous, steady state manner.

Abstract: The isotopes of zirconium can be partially or completely separated by loading an aqueous solution of an ionic compound of zirconium onto a cationic exchange resin which serves as the stationary phase of a chromatograph, eluting the compound with an aqueous acid and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the eluant is a strong mineral acid, such as hydrochloric acid and the chromatograph is of a type, such as a continuous annular chromatograph that it can be operated in a continuous, steady state manner.

Abstract: The isotopes of zirconium can be partially or completely separated by loading an essentially anhydrous alcoholic solution of an ionic compound of zirconium onto a cationic exchange resin with pentavalent phosphorus derived active groups which serves as the stationary phase of a chromatograph, eluting the compound with an essentially anhydrous alcoholic solution of hydrogen chloride and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the active groups of the cation exchange resin are derived from di-2-ethylhexyl phosphoric acid, tri-n-octyl phosphine oxide or tributyl phosphate and the chromatograph is of a type, such as a continuous annular chromatograph that it can be operated in a continuous steady state manner.

Abstract: Continuous production of zirconium and/or hafnium metal from a fused salt bath in which one of the salts is zirconium and/or hafnium tetrachloride is carried out by feeding additional, make-up zirconium and/or hafnium tetrachloride powder into a zirconium and/or hafnium dissolution area of the bath maintained at a dissolution temperature below which the tetrachloride will vaporize, by circulating portions of the bath into and through a separate but contiguous area maintained at a temperature at which the tetrachloride will vaporize, and by recovering the vaporized tetrachloride. It is preferred that the vaporization area of the bath be wholly surrounded by and insulated from the dissolution area of the bath.

Abstract: This is a method of reducing zirconium chloride to a metal product by introducing zirconium chloride into a molten salt bath containing at least one alkali metal chloride and at least one alkaline earth metal chloride; and electrochemically reducing alkaline earth metal chloride to a metallic alkaline earth metal in the molten salt bath, with the reduced alkaline earth metal reacting with the zirconium chloride to produce zirconium metal. By using this electrochemical-metallothermic reduction, zirconium metal is produced and insoluble subchlorides of zirconium in the metal product are generally avoided.Preferably, the molten salt in the molten salt bath consists essentially of a mixture of lithium chloride, potassium chloride, magnesium chloride and zirconium or hafnium chloride.

Abstract: Improvements are described to a process in which the extractive distillation separation of zirconium or hafnium may be accomplished using mixtures of fused alkali metal or alkali metal and alkaline earth chlorides as the solvent. The solvent composition is adjusted to provide a low-melting eutectic, permitting recirculation of the stripped solvent in the liquid phase, as well as reducing the temperature required for thermal stripping (reducing the corrosivity of the fluid). Stripping of the bottoms is accomplished at least partially by direct electrolysis of the bottoms stream, producing the zirconium-free salt recycle stream to be transferred to the top of the column, and at least partially eliminating the need for chemical reduction of the tetrachlorides to metal (a costly process generating undersirable waste streams). Regeneration of the reflux is accomplished in a presurized condenser system, of one or more stages, with all material transport to be done in either the liquid or vapor states.

Abstract: This is a method for molten salt systems related to distillation for zirconium-hafnium separation and prevents buildup of iron chloride by electrochemically reducing iron from the molten salt to give very low levels of iron chloride in the distillation column, to reduce corrosion, improve the product and, in some cases, to allow the molten salt system to be run continuously. The improvement comprises electrochemical purification of molten salt containing zirconium-hafnium chloride either, prior to introduction of the zirconium-hafnium chloride into a distillation column, or after introduction, or both, to substantially eliminate iron chloride from the zirconium-hafnium chloride. The molten salt during the electrochemical purification consists essentially of a mixture of chlorides of alkali metals, alkaline earth metals, zirconium, hafnium, aluminum, manganese, and/or zinc.

Abstract: This is an improved method for separating hafnium from zirconium of the type where a complex of zirconium and hafnium chlorides and phosphorus oxychloride is prepared from zirconium-hafnium chloride and the complex is introduced into a distillation column, with the improvement comprising: electrochemical breaking of the zirconium of hafnium chloride complex taken from said distillation column to separate product from the complex. The electrochemical breaking of the complex, possibly by reducing zirconium or hafnium, is done in a molten salt bath. Preferably, the molten salt in said molten salt bath consists principally of a mixture of alkali metal and alkaline earth metal chlorides and zirconium or hafnium chloride. The product can be either chloride, metal, or mixed metal and subchloride for further processing.

Abstract: This is a zirconium-hafnium separation process utilizing a complex of zirconium-hafnium chlorides and phosphorus oxychloride. The complex is introduced into a distillation column and a hafnium chloride enriched stream is taken from the top of the column and a zirconium chloride enriched stream is taken from the bottom of the column. In particular, the invention utilizes prepurification of the zirconium-hafnium chlorides prior to introduction of the complex into the distillation column to substantially eliminate iron chloride; thus, the buildup of iron chloride in the distillation column is substantially eliminated and the column can be operated in a continuous stable, and efficient manner.

Abstract: A method of purificating titanium tetrachloride, comprising: heating a loose mass of catalytic metal to a temperature over 300.degree. C. approximately, introducing vapor of a crude titanium tetrachloride to contact with said metal, said chloride comprising a minor amount of metal oxychloride, causing a reaction to convert a substantial part of the oxychloride to substances which are less volatile than titanium tetrachloride, removing such substances in condensed state from the titanium tetrachloride in fluid state, and recovering thus purified titanium tetrachloride.

Abstract: This is a molten salt extractive distillation process for separating hafnium from zirconium. It utilizes at least principally a ZnCl.sub.2 --Ca/MgCl.sub.2 molten salt solvent, and preferably ZnCl.sub.2 --Ca/MgCl.sub.2 in a near 95-15 mixture. The extraction column is preferably run about 380.degree.-420.degree. C. at about one atmosphere and stripping is preferably done at about 385.degree.-450.degree. C. utilizing an inert gas carrier.

Abstract: This is a molten salt extractive distillation process for separating hafnium from zirconium. It utilizes at least principally a ZnCl.sub.2 -PbCl.sub.2 molten salt solvent, and preferably ZnCl.sub.2 -PbCl.sub.2 in a near eutectic or eutectic mixture. The extraction column is preferably run about 370.degree.-390.degree. C. at about one atomosphere and stripping is preferably done at 375.degree.-400.degree. C. utilizing an inert gas carrier.

Abstract: There is disclosed, in a process for separating zirconium and hafnium, an improvement for the removal of sodium sulfate from a sulfate-containing sodium chloride solution. This improvement includes adding a water-miscible organic precipitant such as methanol, ethanol or acetone to the sulfate-containing sodium chloride solution. The precipitant is added in an amount sufficient to cause the removal of sulfate as sodium sulfate. The organic precipitant is removed and the substantially sulfate ion free sodium chloride solution is recycled. Also provided is a process for the recovery of sodium sulfate having a purity greater than 99.9%.

Abstract: Separation of zirconium and hafnium by solvent extraction with a tertiary amine from sulfuric acid solution is improved by addition of water-soluble .alpha.-hydroxycarboxylic acid to the aqueous phase.

Abstract: The titanium and zirconium-based minerals, present in the first stage centrifuge tailings from the hot water process for extraction of bitumen from bituminous sands, may be concentrated by a dry screening process. The tailings are burned off to provide a dry, essentially carbon-free, mineral mixture. By screening the mixture into three streams of different particle size range, silica and clays may be rejected as coarse and fine materials respectively, while titanium and zirconium minerals may be concentrated in the intermediate stream. The titanium and zirconium concentrate stream may be advanced to high tension and magnetic separation steps known in conventional processing of heavy minerals, for further beneficiation.

Abstract: A method of essentially preventing the formation of 3-mercapto-4-methyl-2-pentanone by selectively controlling an ammonium thiocyanate-methyl isobutyl ketone regeneration system by maintaining the pH in the range of 4 to 9, and the temperature below 150.degree. F.

Abstract: Titanium dioxide component is removed from a mineral containing titanium dioxide component which is difficult to be separated by the conventional electrostatic separation.In the electrostatic separation from the mineral containing titanium dioxide component, the mineral is pretreated by a heat-treatment in an atmosphere of reducing, neutral or inert gas or a mixture thereof so as to change the electrostatic property of titanium dioxide and separating by an electrostatic separation.

Abstract: A method for the separation of a light reactive metal (e.g., zirconium) from a heavy reactive metal (e.g., hafnium) by forming insoluble nitrides of the metals in a molten metal solvent (e.g., copper) inert to nitrogen and having a suitable density for the light metal nitride to form a separate phase in the upper portion of the solvent and for the heavy metal nitride to form a separate phase in the lower portion of the solvent. Nitriding is performed by maintaining a nitrogen-containing atmosphere over the bath. The light and heavy metals may be an oxide mixture and carbothermically reduced to metal form in the same bath used for nitriding. The nitrides are then separately removed and decomposed to form the desired separate metals.

Abstract: The invention relates to a process for the separation of zirconium, and hafnium tetrachlorides from mixtures thereof. The process according to the invention consists of selectively absorbing zirconium tetrachloride and hafnium tetrachloride vapors in a solvent medium circulating counter-current to these vapors in a distillation column, wherein the solvent consists of a molten chloroaluminate and/or chloroferrate of potassium. The process described may be used to obtain hafnium-free zirconium tetrachloride which may then be used to prepare nuclear-grade zirconium, and hafnium tetrachloride containing little zirconium.

Abstract: A process is provided for separating zirconium and hafnium tetrachlorides by the direct distillation from their solution in an eutectic mixture of sodium and potassium chlorides. Hafnium tetrachloride and zirconium tetrachloride are provided in adequate purity for direct introduction into reduction units for the production of the respective metals by virtue of controlled ratios of the salt eutectic solvent to the hafnium and zirconium tetrachlorides and by provision of a reflux of hafnium with added increments of the eutectic solvent salt mixture.