Abstract: Method for reduction in metallic impurities in aqueous and anhydrous TiCl.sub.4. The method utilizes activated carbon to remove poisonous impurities such as antimony and arsenic, which allows use of the TiCl.sub.4 in pearlescent pigment production and cosmetics.

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: An improved process for the preparation of TiCl.sub.4 comprising(a) chlorinating a raw material containing titanium and vanadium impurities to produce a crude TiCl.sub.4 reaction product,(b) separating the crude reaction product into solid by-products and TiCl.sub.4 -containing liquid,(c) reacting the TiCl.sub.4 -containing liquid with a reducing agent whereby vanadium impurities are converted into solid compounds, and(d) separating TiCl.sub.4 from the solid vanadium compounds, is improved by adding solid products of the vanadium reduction reactions to the crude TiCl.sub.4 reaction product prior to the separating step (b).

Abstract: The present invention relates to a method of producing a fluoride glass preform and/or fiber having a modified refractive index by heating the fluoride glass preform to a temperature that is above its glass transition temperature, but below its devitrification temperature; inserting a first electrode into the inner core of the preform and surrounding the outer perimeter of the preform with a second electrode of opposite polarity; means for generating an electromotive force; and applying an electromotive force through the first electrode and the second electrode which causes a movement of positive ions toward the electrode of opposite charge while simultaneously causing a movement of negative ions toward its electrode of opposite charge such that the movement of these ions results in a modification of the refractive index of the preform.

Abstract: The invention relates to an apparatus for preparing tantalum halide supported catalysts which comprises a container for holding the support, a container for holding the tantalum pentahalide, a heating means to provide the proper temperature for reactive sublimation, and an optional means for transferring vapor from the halide container.

Abstract: Heavy metal fluoride glasses are made by a process that requires high purity fluoride constituent compounds, some of which are further refined by sublimation. Handling occurs in a protective atmosphere such as argon. The charge is placed in a sealed modified optical growth furnace having the ability of atmosphere control, heat control and position control of the charge. The charge is firstly raised to its fusion temperature, then to an admixture temperature, and finally to a higher temperature. The charge is immediately removed from the heating source and quickly cooled through the critical crystallization region. The total heating and cooling time being about one to two hours. The resulting glass ingot is partially annealed. The HMFG of (Zr or Hf)F.sub.4 -BaF.sub.2 -LaF.sub.3 -AlF.sub.2 consistently exhibits low levels of both light scattering and bulk OH contact, along with very reproducible hardness, thermal parameters, and UV and IR edge absorption behavior.

Abstract: Metal halide particles useful, among other things, as olefin polymerization catalyst precursors and catalyst supports are prepared by vaporizing the metal halide and then condensing it in the presence of a diluent.

Abstract: Chlorine may be recovered from residues from the fluidized bed chlorination of iron-containing metalliferous oxidic materials, such as ilmenite, bauxite, chromite, wolframite, scheelite, tantalite or columbite, the residues containing condensed iron chloride and blow-over bed solids, by heating the residue to revolatalize the iron chloride and reacting it with oxygen. The quantity of iron chloride in the oxidic material is controlled relative to the quantity of blow-over carbon so that the quantity of carbon is sufficient on combustion to provide the required heat but is insufficient to cause undue dilution of the chlorine produced by virtue of its combustion products. Chlorine of a concentration suitable for direct recycle to a chlorination process, e.g. of 30% to 50% volume concentration is produced.

Abstract: The present invention relates to an electrolysis bath based on trivalent chromium.This bath is characterized in that it contains a trivalent chromium halide which is neither chelated by a chelating product of chromium nor accompanied by a special organic solvent.Due to simple operational characteristics, this bath makes it possible to obtain commercially interesting results since, with respect to the color, thickness and hardness of the deposits obtained, very close to those of conventional baths based on hexavalent chromium, this with the advantage, over the latter, of having a speed and a yield of deposit which are much greater and conditions of use which are less toxic and less polluting.

Abstract: A process is disclosed for recovering cobalt in a relatively pure form from an impure cobalt bearing material. The process involves digesting the material in hydrochloric acid to form a solution essentially all of the cobalt and some impurities and insoluble material containing the remainder of the impurities, separating the solution from the insolubles, adding an oxalate producing compound in an amount sufficient to subsequently convert essentially all of the cobalt to cobalt oxalate to the solution, adjusting the pH of the oxalate treated solution to from about 1.5 to about 2.0 with a base to precipitate the cobalt, and finally separating the precipitate from the resulting mother liquor.

Abstract: A process is described for reacting chlorinated, nitrogen-containing hydrocarbons with metal oxides so as to convert essentially all of the carbon atoms to oxides of carbon. This process provides an efficient and economically valuable use for chlorinated, nitrogen-containing hydrocarbons.

Abstract: A method for preparing ultra-pure metal tetrafluorides in which 3d such as Fe impurities are separated from impure material by a combined vaporization-electrolytic separation procedure. Sublimation and distillation methods are disclosed in combination with electrolytic separation by both emf-series displacement (ESD) and direct melt electrolysis (DME).

Abstract: A process for the beneficiation of an iron-containing material is carried out by first chlorinating the iron-containing material. Oxidation of ferrous chloride in the effluent gas from the chlorination is carried out under controlled conditions of oxygen supply so that more than 50% but less than 100% of the ferrous chloride is oxidized. In this way chlorine gas is separated from the process stream in a relatively pure form which can be utilized in a continuous process by recycle to another chlorination.

Abstract: A selective chlorination method of a mixture of simple or complex metallic oxides, comprising at least one of the elements to be used, iron, aluminum, titanium and silicon, as well as the impurities accompanying said elements, said method consisting of a grinding, a calcination, a placing in suspension in a bath of melted salts of the mixture of said metallic oxides and of their impurities and of an introduction of chlorinating agents into said bath maintained at a temperature which assures the volatility of at least one of the metallic chlorides formed; characterized by the fact that, in order to selectively extract the metallic chlorides formed from the bath, specific chlorinating mixtures are introduced into this bath by successive steps, said mixtures having increasing chlorinating power, and the introduction is in a number at the most equal to the usuable elements to be chlorinated.

Abstract: A process for preparing solid titanium trichloride useful for the polymerization of an .alpha.-olefin, which comprises precipitating violet-colored fine solid particles of titanium trichloride at a temperature of not higher than 150.degree. C. from a liquid of titanium trichloride liquefied in the presence of an ether, characterized in that after the amount of the precipitated violet-colored fine solid particles of titanium trichloride reaches at least 80% based on the total amount of titanium trichloride in the system, titanium tetrachloride is added in an amount within a molar ratio of from 0.2 to 10 based on the total amount of titanium trichloride in the system, followed by aging at a temperature of from 60.degree. to 120.degree. C.

Abstract: Molten alkaline earth metal halides are used to convert highly stable oxides into the corresponding anhydrous halides. Usually a third reactant, such as silica, is added in order to bind the basic oxide thus formed. The solid oxide compounds (e.g. silicates) which result are wellknown ceramic phases of a high degree of purity.

Abstract: A process of preparing chromium (III) compounds from chromate and/or dichromate salts by forming a mixture of such salts, an acid, water and a reducing agent. Additional acid is added to the mixture which is then cooled selectively precipitating the salt of the anion of the acid and the cation of the chromate and/or dichromate salts which is separated from the solution containing the desired chromium (III) compound.

Abstract: Finely-divided titanium diboride or zirconium diboride powders are formed by reacting gaseous boron trichloride with a material selected from the group consisting of titanium powder, zirconium powder, titanium dichloride powder, titanium trichloride powder, and gaseous titanium trichloride.

Abstract: An organometallic halide having the formula:(RMX) (MX.sub.2).sub.a (MR.sub.2).sub.b (MH.sub.2).sub.cwherein a.ltoreq.0.45, b.ltoreq.0.15, and c.ltoreq.0.30, X is a halogen, R is a hydrocarbon radical, and M is a metal selected from the group consisting of magnesium, zinc, beryllium, and calcium is prepared by a continuous dry process by reacting an organic monohalide RX and a metal M in the form of convex solid grains of a size between 1 and 15 mm. The reaction temperature is lower than the temperature at which decomposition of the organometallic halide RMX begins and at least 10.degree. C. higher than the boiling point of the organic monohalide. The reaction may also take place in the presence of an organometallic derivative comprising a hydroxy group or an enolysable ketone group. The resulting organometallic halide may be used for the synthesis of anhydrous magnesium halide or for the reduction of titanium tetrachloride.

Abstract: Components of catalysts for polymerizing olefins having the general formula:VCl.sub.n (OR).sub.min which R=a hydrocarbon radical having 1-18 C; or R.sub.p.sup.1 Si(OH).sub.3-p, in which R.sup.1 =a hydrocarbon radical, 1.ltoreq.p.ltoreq.3; 1.5.ltoreq.n.ltoreq.3, m=3-n; with X-ray powder spectrum, in which maximum intensity diffraction lines, which in the spectrum of normal VCl.sub.3 appear at d=5.75 .ANG., d=2.67 .ANG. and d=1.74 .ANG., exhibit a broadening of the half peak breath of at least three times for the diffraction line at d=5.75 .ANG. and of at least four times for the diffraction lines appearing at d=2.67 .ANG. and d=1.74 .ANG., or said diffraction lines disappear.

Abstract: A method for removing oxide contamination from titanium diboride powder involves the direct chemical treatment of TiB.sub.2 powders with a gaseous boron halide, such as BCl.sub.3, at temperatures in the range of 500.degree.-800.degree. C. The BCl.sub.3 reacts with the oxides to form volatile species which are removed by the BCl.sub.3 exit stream.

Abstract: A process is described for reacting chlorinated hydrocarbons other than carbon tetrachloride with metal oxides so as to convert essentially all of the carbon atoms to oxides of carbon. This process provides an efficient and economical means for utilizing chlorinated hydrocarbons.

Abstract: A method is described for the preparation of high surface area metal fluorides and metal oxyfluorides comprising reacting high surface area metal oxides with a fluorocarbon vapor wherein the fluorocarbon is selected from the group consisting of CH.sub.4-Q F.sub.Q wherein Q is 1 to 3 and totally or partially fluorinated C.sub.2 -C.sub.6 alkanes, alkenes and alkynes and C.sub.5 -C.sub.6 cyclic alkanes, preferably fluoroform (CHF.sub.3) wherein the metal oxides and the fluorocarbon vapors are contacted at a temperature of from about 300.degree. to about 800.degree. C., for a time sufficient to effect the essentially complete conversion of the metal oxides into metal fluorides or the partial conversion of the metal oxides into metal oxyfluorides.

Abstract: In a process for producing a titanium trihalide by reducing a titanium tetrahalide with hydrogen, the improvement wherein the reduction is carried out in an organic solvent in the presence of an ether and at least one member of the group consisting of metals of Groups IB, IIB, IVB and VIII of the periodic table and compounds of these materials.

Abstract: A method for imparting ductility and very high electrical conductivity to very brittle refractory single crystals by subjecting said crystals to a hydrostatic deformation technique at room temperature and at pressures of from about 5 to 25 kilobars.

Abstract: The chlorides of elements of Groups III, IV and V of the Periodic Table, such as, boron trichloride, silicon tetrachloride, zirconium tetrachloride and vanadium tetrachloride are prepared by heating activated carbon particles having a supported aqueous solution of compounds of the elements of Groups III, IV and V of the Periodic Table thereon at a temperature of from 300.degree. through 1000.degree. C. and, then, reacting the resultant activated carbon particles with chlorine.

Abstract: A fine solid titanium trichloride is used as a catalyst for a polymerization of an .alpha.-olefin. The solid titanium trichloride is produced by precipitating it at lower than 150.degree. C. from a liquid titanium trichloride complex in the presence of an ester having the formula ##STR1## wherein R.sup.1 and R.sup.2 respectively represent a hydrocarbon moiety and total carbon atoms of R.sup.1 and R.sup.2 are 10 or more.

Abstract: An improved method of extracting titanium from titaniferous materials by reaction with thionyl chloride to form titanium tetrachloride which is separated from the reaction products by volatilization or by extraction.

Abstract: The process is based on the series of halide-forming affinities. The oxides are passed through a series of zones equal in number to the plurality of halides or mixtures which are to be produced. A halide of an element of lower halide-forming affinity is fed counter-current to the oxides. The halide supply is in stoichiometric equivalent to the total content of halide to be extracted. The oxide of the said fed element is also extracted.

Abstract: Vanadium impurities in chlorinated titaniferous materials are rendered easily removable by reacting said chlorinated titaniferous materials with a high surface area carbon at an elevated temperature. A process for preparing said high surface are a carbon is also described.

Abstract: A method is described for the preparation of high surface area metal fluorides and metal oxyfluorides comprising reacting high surface area metal oxides with a fluorocarbon vapor wherein the fluorocarbon is selected from the group consisting of CH.sub.4-Q F.sub.Q wherein Q is 1 to 3 and totally or partially fluorinated C.sub.2 -C.sub.6 alkanes, alkenes and alkynes and C.sub.5 -C.sub.6 cyclic alkanes, preferably fluoroform (CHF.sub.3) wherein the metal oxides and the fluorocarbon vapors are contacted at a temperature of from about 300.degree. to about 800.degree. C., for a time sufficient to effect the essentially complete conversion of the metal oxides into metal fluorides or the partial conversion of the metal oxides into metal oxyfluorides.

Abstract: A method of producing aluminum chloride from aluminous materials containing compounds of iron, titanium and silicon comprising reacting the aluminous materials with carbon and a chlorine-containing gas at a temperature of about 900.degree. K. to form a gaseous mixture containing chlorides of aluminum, iron, titanium and silicon and oxides of carbon; cooling the gaseous mixture to a temperature of about 400.degree. K. or lower to condense the aluminum chlorides and iron chlorides while titanium chloride and silicon chloride remain in the gas phase to effect a separation thereof; heating the mixture of iron chlorides and aluminum chlorides to a temperature of about 800.degree. K. to form gaseous aluminum chlorides and iron chlorides; passing the heated gases into intimate contact with aluminum sulfide to precipitate solid iron sulfide and to form additional gaseous aluminum chlorides; and separating the gaseous aluminum chloride from the solid iron sulfide.

Abstract: A method of forming the chloride of a metal-oxygen-containing substance, including the steps of coating particles of such substance with green carbon, i.e. carbon which contains substances more volatile than carbon, heating the coated particles to drive off the volatile matter and produce openings such as pores and fissures, and then reacting the particles from the step of heating with a source of chlorine.

Abstract: This invention relates to a process for selectively recovering vanadium from spent catalysts which were used in hydrodesulufurization, hydrodemetallization, etc. of heavy oils until metals in said heavy oils accumulated thereon. More particularly, it relates to a process for recovering vanadium, and if desired, vanadium along with nickel from spent catalysts in such a way that said spent catalysts are chlorinated with chlorinating agent(s) at a temperature below 600.degree. C. without being subjected to calcination so as to convert almost all the vanadium compounds to vanadium tetrachloride which is recovered in the form of a gas, including the chlorination of nickel compounds of nickel chloride which can also be recovered as such by solvent extraction.

Abstract: Particles of titanium trichlorides usable for the stereospecific polymerization of alpha-olefines, especially propylene, having been dried until their liquid content is less than 1% by weight relative to the weight of titanium trichloride present in said particles, as well as a process for the preparation of such particles and a process for stereospecific polymerization in the presence thereof.

Abstract: The stability of vanadium tetrachloride is improved by the addition of phosphorus trichloride such as phosphorus trichloride. Preferably, the vanadium tetrachloride is provided by the reductive chlorination of vanadium oxychloride in the presence of activated carbon having a sulfur content less than 1% by weight.

Abstract: A process for the preparation of violet TiCl.sub.3 by reducing TiCl.sub.4 with an organo-aluminum compound, characterized in that:(a) the TiCl.sub.4 is premixed with a complexing agent in an inert organic solvent, the molar ratio complexing agent:TiCl.sub.4 being within the range from 0.3:1 to 2:1;(b) the organo-aluminum compound is premixed with a complexing agent in an inert organic solvent, the molar ratio complexing agent:organo-aluminum compound being at least 0.25:1;(c) the reduction to TiCl.sub.3 and precipitation of TiCl.sub.3 are carried out by combining at least one stoichiometric equivalent of TiCl.sub.4 in the premixed composition of step (a) with one stoichiometric equivalent of the organoaluminum compound in the premixed composition of step (b) over a period of less than one hour at a temperature within the range 60.degree. to 110.degree. C.; and(d) the final concentration of violet TiCl.sub.3 in the reaction mixture is at least 0.2 mol./liter.

Abstract: In the conversion of a metal oxide to a metal chloride by reaction with chlorine and carbon monoxide wherein hydrogen chloride is produced as byproduct, the byproduct hydrogen chloride is contacted with a molten salt mixture containing the higher and lower valent chlorides of a multivalent metal and oxygen to recover the hydrogen chloride by enriching the salt in the higher valent metal chloride. Essentially all of the chlorine values are recovered from the salt by direct contact with all or a portion of the carbon monoxide fresh feed to the metal chloride production, with such carbon monoxide stripping gaseous chlorine from the salt, as well as combining with the chlorine to produce phosgene. The carbon monoxide, chlorine and phosgene are employed in the metal chloride production.

Abstract: Ferruginous titaniferous material is chlorinated with chlorine for producing a product stream of titanium chlorides and by-product metallic iron in a laminar flow process.

Abstract: A process is disclosed for recovering metallic constituents of spent or waste catalysts containing metallic compounds fixed on an aluminous support. The process is particularly applicable for the recovery of metals such as Al, Mo, V, Ni and Co, contained in spent catalyst. The process comprises transforming the metals to be recovered into volatile chlorides by carbochlorination and then separating the chlorides obtained by dry means and fixing them successively in a selective manner. The separation of AlCl.sub.3 is accomplished by passage through granules of anhydrous NaCl, and the separation of MoCl.sub.5 by passage through granules of crystallized KCl. The process is particularly suitable for the treatment of waste catalyst from the catalytic hydrocracking or hydrodesulfurization of oils.

Abstract: A process for forming a metal chloride of a metal or its compound comprising forming a liquid fused salt bath mixture of at least two metal chlorides, the bath having the property of dissolving the formed metal chloride, and introducing the metal or compound into the liquid fused salt bath in the presence of chlorine to form the metal chloride and recovering the formed chloride from the liquid fused salt bath mixture. The metals which may be chlorinated are those from groups 1b, 2a, 2b, 3a, 3b, 4a, 5a and 8 of the periodic table and the rare earth metals. Compounds from which the metals may be chlorinated are the sulfides, oxides, carbonates and sulfates. Chlorine may be introduced as such or its source may be a chlorine donor such as ferric chloride or sulfur chloride. The chlorides for the liquid fused salt bath are those of alkali metals, alkaline earth metals, ammonia, zinc, and ferric iron. The chlorination can be performed within a temperature range of 150.degree. C.-1000.degree. C.

Abstract: Product yields are increased and effluent streams purified for disposal by an improved process for producing vanadium chlorides. The process comprises reacting vanadium oxide with chlorine and reactant carbon to produce substantially pure vanadium chlorides and an effluent stream containing vanadium chlorides and unreacted chlorine. The effluent stream is contacted with adsorptive carbon whereby the vanadium chlorides and chlorine are adsorbed thereon. The adsorptive carbon is subsequently recycled and used as the reactant carbon.

Abstract: Titanium trichloride which is obtained during one step of a process for recovering titanium metal values from a titanium bearing source which still contains some impurities such as iron and vanadium compounds may be purified by drying the titanium compound in an air atmosphere, further drying under a carbon monoxide atmosphere and thereafter roasting the dried compound in the presence of chlorine at an elevated temperature to separate the impurities from the desired titanium compounds.

Abstract: A process for the removal of aluminum chloride from a liquid solution thereof with the liquid metal chlorides resulting from the chlorination of titaniferous materials by mixing water and sodium chloride with the liquid solution in amounts such that the amount of water is less than equimolar with respect to the total amount of aluminum chloride and the combined amount of water and sodium chloride is at least equimolar with respect to the total amount of aluminum chloride. This process significantly decreases the corrosion of apparatus associated with the presence of aluminum chloride and substantially eliminates losses of titanium tetrachloride and ferric chloride present in the liquid solution and reduces the formation of HCl.

Abstract: Anhydrous TaF.sub.5 can be synthesized from a mixture comprising water and fluorotantalic acids by contacting said mixture with a dehydrating agent. Preferably, said mixture is formed by contacting tantalum oxides, tantalum oxide-halides or mixtures thereof with HF. The dehydrating agent should be a compound that contains carbon-chlorine bonds, carbon-bromine bonds or mixtures thereof.

Abstract: A process for the manufacture of a titanium-containing component of a catalyst for the polymerization of monoolefins by the Ziegler-Natta method by milling (a) a titanium trichloride/aluminum trichloride complex and (b) a particular ether with one another, in which process (1) a vibratory ball mill producing a particular milling acceleration is used, (2) until from 6 to 85% of the aluminum trichloride originally present in a bonded form in the titanium-containing compound (a) have been eliminated from the said compound (a). Polyolefins of high stereoregularity can be obtained in a high specific yield by means of the catalyst component manufactured according to the invention.

Abstract: Solid titanium trichloride in the form of fine granules having low aluminum compound content, which is suitable as a catalyst for polymerization of .alpha.-olefins, especially, propylene is obtained as a precipitate by heating liquefied titanium trichloride in the presence of a liberating agent, and separating the thus formed precipitate. The liquefied titanium trichloride is preferably prepared with an reducing titanium tetrachloride by organic aluminium compound in the presence of ether and hydrocarbon.

Abstract: Solid titanium trichloride in the form of fine granules having low aluminum compound content, which is suitable as a catalyst for polymerization of .alpha.-olefins, especially, propylene is obtained as a precipitate by heating liquefied titanium trichloride in the presence of a liberating agent, and separating the thus formed precipitate. The liquified titanium trichloride is preferably prepared with an reducing titanium tetrachloride by organic aluminum compound in the presence of ether and hydrocarbon.