Forming Metallic Iron Or Insoluble Iron Containing Compound Patents (Class 423/83)
  • Patent number: 9212066
    Abstract: Processes of preparing metal titanate from one or more metal compounds, and a product provided by the process. In one embodiment, sodium titanate and an ionic metal compound are mixed into an aqueous mixed slurry, which is allowed to react into metal titanate at the boiling point of the mixed slurry or below, by mixing it at normal pressure and in a normal gaseous atmosphere. After this, the metal titanate product is optionally washed, and/or filtered and dried.
    Type: Grant
    Filed: November 4, 2008
    Date of Patent: December 15, 2015
    Assignee: SACHTLEBEN PIGMENTS OY
    Inventors: Ralf-Johan Lamminmäki, Jani Kallioinen, Arja-Leena Ruohonen
  • Patent number: 9175367
    Abstract: A process for neutralization is provided which can maintain a high solid content of a bauxite dissolution residual substance slurry even after a neutralization treatment is completed and the stabilize pH within a short time of the neutralization treatment. Such a process for neutralizing a bauxite dissolution residual substance containing a desiliconizing product which is generated in the production process of aluminum hydroxide using Bayer process, includes: mixing a bauxite dissolution residual substance or a bauxite dissolution residual substance slurry with sulfuric acid in an amount ranging from 0.6 to 1.2 equivalence to the total amount of sodium contained in the bauxite dissolution residual substance or a bauxite dissolution residual substance slurry, such that the solid content after mixing becomes 400 to 700 g/l to gelate the mixture, and thereafter obtaining a bauxite dissolution residual substance neutralized slurry.
    Type: Grant
    Filed: March 7, 2014
    Date of Patent: November 3, 2015
    Assignee: SHOWA DENKO K.K.
    Inventor: Isao Ishikawa
  • Patent number: 8912111
    Abstract: A process for slurry hydrocracking catalyst recovery is described. In one embodiment, the process includes separating effluent from a slurry hydrocracking zone into a first portion comprising solvent and clarified pitch and a second portion comprising pitch and catalyst. The second portion is contacted with an acid to leach the catalyst out of the pitch forming an aqueous solution and pitch residue. The aqueous solution is contacted with an anion to form an insoluble salt which is the catalyst.
    Type: Grant
    Filed: August 7, 2012
    Date of Patent: December 16, 2014
    Assignee: UOP LLC
    Inventors: Rajeswar R. Gattupalli, Grant H. Yokomizo, Bart Dziabala
  • Patent number: 8728437
    Abstract: A sulfate process for producing titania from a titaniferous material (as herein defined) including a step of leaching said titaniferous material with a leachant to form a process solution that includes an acidic solution of titanyl sulfate and iron sulfate, wherein said sulfate process further includes a filtration step comprising filtering said leachant to at least substantially remove titanyl sulfate particles from said leachant prior to supplying said leachant to said leach step.
    Type: Grant
    Filed: September 29, 2009
    Date of Patent: May 20, 2014
    Assignee: BHP Billiton Innovation Pty Ltd
    Inventors: Alan David Stuart, John Andrew Lawson, Christopher Brett Ward, Hong Peng
  • Publication number: 20110229386
    Abstract: A sulfate process for producing titania from a titaniferous material (as herein defined) including a step of leaching said titaniferous material with a leachant to form a process solution that includes an acidic solution of titanyl sulfate and iron sulfate, wherein said sulfate process further includes a filtration step comprising filtering said leachant to at least substantially remove titanyl sulfate particles from said leachant prior to supplying said leachant to said leach step.
    Type: Application
    Filed: September 29, 2009
    Publication date: September 22, 2011
    Inventors: Alan David Stuart, John Andrew Lawson, Christopher Breff Ward, Hong Peng
  • Patent number: 7943103
    Abstract: A process is provided for handling waste solids produced from the chlorination of titanium-bearing ores in the presence of coke as a reducing agent. The process includes the steps of combining waste metal chloride solids and unreacted ore and coke solids with a liquid whereby waste metal chloride solids are dissolved in the liquid and unreacted ore and coke solids are slurried in the liquid, and separating out the unreacted ore and coke solids from the liquid. The liquid including the dissolved waste metal chlorides is then divided into a recycle substream and a bleed substream. The recycle substream is recycled such that it comprises at least a part of the liquid which is combined with the waste metal chloride solids and unreacted ore and coke solids in the product stream. The bleed substream is neutralized to produce a filterable or directly landfillable mass of waste metal hydroxide solids.
    Type: Grant
    Filed: April 27, 2006
    Date of Patent: May 17, 2011
    Assignee: Tronox LLC
    Inventors: Harry E. Flynn, Leslie E. Crowder
  • Patent number: 7931886
    Abstract: According to the present invention there is provided a process for the agglomeration of titania slag particles comprising providing titania slag at a d50 particle size of below 106 ?m; mixing the slag particles with an organic binder; and agglomerating the mixture of the slag particles and organic binder into agglomerated particles with a d50 particle size in the range from 106 ?m to 1000 ?m. The agglomerated particles have a (TiO2 and FeO)/C mass ratio of more than 3.4. The invention also relates to such agglomated slag particles and a chloride process for the production of TiO2 wherein such agglomerated titania slag particles are used.
    Type: Grant
    Filed: September 14, 2005
    Date of Patent: April 26, 2011
    Assignee: Kumba Resources Limited
    Inventors: Pieter Adriaan Botha, Gert Hendrik Jacobus Coetzee, legal representative, Deon Bessinger, Benjamin Alexander Dippenaar
  • Publication number: 20090311153
    Abstract: A sulfate process for producing titania from a titaniferous material (such as an iron-containing titaniferous material such as ilmenite) is disclosed. The process includes digestion and/or leach steps that form a process solution that includes an acidic solution of titanyl sulfate (TiOSO4) and iron sulfate (FeSO4) from the solid titaniferous material. The process also includes hydrolysis and other steps that form titania from the titanyl sulfate in the process solution. The process is characterised by a ferric ion treatment step of treating the process solution and lowering the concentration of ferric ions from the process solution.
    Type: Application
    Filed: September 6, 2007
    Publication date: December 17, 2009
    Inventors: Eric Girvan Roche, Philip Ernest Grazier, Alan David Stuart
  • Patent number: 7618601
    Abstract: A process for the enrichment of anatase mechanical concentrates, in order to obtain synthetic rutile with low contents of rare earth and radioactive elements, comprising the steps of: calcination of the anatase concentrate; reduction of the calcined product; dry or wet low-intensity magnetic separation of the reduced product; dry, high-intensity, high-gradient magnetic separation of the non-magnetic fraction from the low-intensity separation; leaching of the high-intensity magnetic fraction; oxidation of the dried product; leaching of the quenched product; filtering of the product from the second leaching; drying of the filtered product; and dry, high-intensity, high-gradient magnetic separation of the product of the second leaching.
    Type: Grant
    Filed: September 20, 2006
    Date of Patent: November 17, 2009
    Assignee: Companhia Vale Do Rio Doce
    Inventors: Lino Rodrigues De Freitas, Ronaldo Moreira De Horta, Joao Alberto Lessa Tude
  • Patent number: 7601313
    Abstract: A process of producing 99% plus titanium dioxide product by using conventional and microwave heating and leaching of the titanium compound feedstock using acid and oxidants. The solid residue from the leaching is used to produce the high quality titanium oxide by froth flotation. Hydrochloric acid can be recovered by multi-stage evaporation. The process can be modified to produce nano-size titanium dioxide product.
    Type: Grant
    Filed: October 8, 2002
    Date of Patent: October 13, 2009
    Assignee: RMG Services Pty Ltd
    Inventor: Rodolfo Antonio M Gomez
  • Publication number: 20090252662
    Abstract: The invention relates to a process for purifying inorganic materials by treating the materials with a solution of hydrogen fluoride in aqueous hydrofluorosilicic acid. The process involves treating an inorganic material containing at least two species, to at least partially separate a first species contained in the material from a second species contained in the material, and comprises treating the material with a fluorine acid solution comprising aqueous hydrofluorosilicic acid and hydrofluoric acid (HF), such that the first species is converted to a product selected from the group consisting of a fluoride, a fluorosilicate and mixtures thereof, and such that the second species is at least partly unreacted, and separating the second species from the product.
    Type: Application
    Filed: June 12, 2009
    Publication date: October 8, 2009
    Applicant: ADVORTECH HOLDINGS PTY LTD
    Inventor: Robert Lloyd
  • Patent number: 7572418
    Abstract: A process for production of titanium concentrate with low contents of radionuclide elements from anatase mechanical concentrates. The process involves calcination in air and reduction with hydrogen or any other reducing gas, both in fluidized bed reactor or rotary kiln, low-intensity magnetic separation of the reduced product, high-intensity magnetic separation of the non-magnetic fraction resulting from the low-intensity magnetic separation, hydrochloric acid leaching of the product of high-intensity magnetic separation, filtering and dewatering of the leached product, high temperature oxidation of the dewatered material, cooling of the oxidized ore, hydrochloric acid leaching of the oxidation product in the presence of sodium fluoride, filtration and drying of the product of the second leaching and high intensity magnetic separation, the non-magnetic fraction of this final magnetic separation becoming the end product.
    Type: Grant
    Filed: October 18, 2004
    Date of Patent: August 11, 2009
    Assignee: Companhia Vale do Rio Doce
    Inventors: Ronaldo De Moreira Horta, Lino Rodrigues De Freitas, João Alberto Lessa Tude
  • Publication number: 20090158895
    Abstract: The invention provides a method for the Industrial purification of a titanium feed stream of purity P1, by the formation of a titanium-double-salt precipitate of purity P2 and a titanium solution with purity P3, wherein P2>P1>P3, the method comprising the steps of: i. forming, from the feed, a medium comprising water, titanium ion, a cation selected from the group consisting of ammonium, cations of alkali metals, protons and a combination thereof, and an anion selected from the group consisting of OH, SO4, HSO4, halides and a combination thereof, which formed medium is further characterized by the presence of (a) a double-salt precipitate comprising titanium ion, at least one of the cations and at least one of the anions; and (b) a titanium solution; and wherein the concentration of the anion in the titanium solution is higher than 15% and the ratio between the concentrations of the cation and the anion in the titanium solution is higher than 0.2 and lower than 1.6; and ii.
    Type: Application
    Filed: October 15, 2006
    Publication date: June 25, 2009
    Inventors: Asher Vitner, Aharon Eyal, Revital Mali
  • Publication number: 20080124261
    Abstract: A sulfate process for producing titania from a titaniferous material as disclosed. The process is characterized by a particular step of precipitating titanyl sulfate.
    Type: Application
    Filed: October 8, 2007
    Publication date: May 29, 2008
    Inventors: Eric Girvan Roche, Sarah Nicholson
  • Publication number: 20080124260
    Abstract: A sulfate process for producing titania from a titaniferous material as disclosed. The process is characterized by particular steps of separating precipitated titanyl sulfate from solution and subsequently treating the precipitated material prior to hydrolysis.
    Type: Application
    Filed: October 8, 2007
    Publication date: May 29, 2008
    Inventors: Eric Girvan Roche, Sarah Nicholson
  • Publication number: 20080124262
    Abstract: A sulfate process for producing titania from a titaniferous material as disclosed. The process is characterized by a particular step of precipitating titanyl sulfate from solution.
    Type: Application
    Filed: October 8, 2007
    Publication date: May 29, 2008
    Inventors: Eric Girvan Roche, Sarah Nicholson
  • Patent number: 6692719
    Abstract: A process is disclosed for regenerating an aqueous acid halide leachant from a spent aqueous metal halide leach liquor. The process comprises introducing into a fluidized bed or spray roaster a hydrocarbon fuel, an oxygen-enriched oxidizing gas and the aqueous metal halide leach liquor; pyrohydrolyzing the aqueous metal halide leach liquor by combustion of the hydrocarbon fuel with the oxygen-enriched oxidizing gas to produce an acid halide-containing gas fraction and a metal oxide-containing solid fraction; separating the gas fraction from the solid fraction, recovering heat energy from the acid halide-containing gas fraction and absorbing the gas fraction in water to produce the aqueous acid halide leachant. The oxygen-enriched oxidizing gas has an oxygen concentration of greater than about 21 percent by volume, preferably greater than about 50 percent by volume, more preferably greater than about 80 percent by volume, and even more preferably greater than about 90 percent by volume.
    Type: Grant
    Filed: November 8, 2000
    Date of Patent: February 17, 2004
    Assignee: Hatch Ltd.
    Inventors: Bert Wasmund, Kamal Adham
  • Patent number: 6468483
    Abstract: A method for processing alumina-bearing ores such as bauxite to recover iron, aluminum, silicon and titanium metal values therefrom the method comprising the steps of adding the alumina-bearing ores to a digester containing an acid to provide a mixture of acid and alumina-bearing ores and heating the mixture to dissolve soluble compounds of at least one of iron, aluminum, silicon and titanium to provide a digest containing dissolved salts of the soluble compounds and to provide a gas component. Thereafter, the digest is treated with water to dissolve water soluble salts therein to provide a slurry comprised of a liquid containing water and the dissolved soluble salts and a solid component comprised of silica. The solid component is separated from the liquid and the pH of the liquid is adjusted to form an aluminate and an iron-containing precipitate.
    Type: Grant
    Filed: May 3, 2001
    Date of Patent: October 22, 2002
    Assignee: Goldendale Aluminum Company
    Inventors: Robert J. Barnett, Michael B. Mezner
  • Patent number: 6447738
    Abstract: A process for the extraction of alumina, iron oxide and titanium dioxide from bauxite ore and clays, and other ore bodies and feedstocks. The process starts by sulfuric acid leaching of the feedstocks in pressure autoclaves at about 200° C. and appropriate pressure. A leach liquor of sulfate salts of aluminum, iron and titanium is obtained. Any iron values are converted to a ferrous state. A recycled potassium sulfate helps produce double aluminum alkali sulfate crystals in the reduced leach liquor. The crystals are removed at about 20°-60° C. with the help of SO2 gases that reduce the ferric. Such double salt is hydrolyzed into a basic aluminum alkali precipitated sulfate salt. This is then dried and calcined at about 950° C. Any alkali sulfate is washed out and recycled. The remainder is alumina. The ferrous sulfate is crystallized out at about 10° C. It is dried and calcined at about 450° C. to produce an iron oxide mixed with other sulfate salts that can be washed out and recycled.
    Type: Grant
    Filed: August 24, 2000
    Date of Patent: September 10, 2002
    Assignee: Solv-Ex Corporation
    Inventors: John S. Rendall, Massoud Ahghar, Jerry V. Fox, Fred A. Aiken
  • Patent number: 6248302
    Abstract: A method for processing red mud to recover iron, aluminum, silicon and titanium metal values therefrom the method comprising the steps of adding the red mud to a digester containing an acid to provide a mixture of acid and red mud and heating the mixture to dissolve soluble compounds of at least one of iron, aluminum, silicon and titanium to provide a digest containing dissolved salts of the soluble compounds and to provide a gas component. Thereafter, the digest is treated with water to dissolve water soluble salts therein to provide a slurry comprised of a liquid containing water and the dissolved soluble salts and a solid component comprised of silica. The solid component is separated from the liquid and the pH of the liquid is adjusted to form an aluminate and an iron-containing precipitate.
    Type: Grant
    Filed: February 4, 2000
    Date of Patent: June 19, 2001
    Assignee: Goldendale Aluminum Company
    Inventors: Robert J. Barnett, Michael B. Mezner
  • Patent number: 5997606
    Abstract: A process for producing titanium slag which is low in radioactivity wherein molten titanium slag, produced by smelting ilmenite in the presence of a reductant in a DC electric arc furnace, is separated from molten iron, boron in an amount which is less than 2.5% equivalent B.sub.2 O.sub.3 of the slag is blended with the molten slag which thereafter is allowed to cool to form a glassy phase which contains the bulk of the radioactive elements of the slag before being crushed to particles below about 1 mm, whereafter the radioactive elements are leached to leave a titanium slag product which is low in radioactivity.
    Type: Grant
    Filed: August 6, 1998
    Date of Patent: December 7, 1999
    Assignee: Billiton SA Limited
    Inventors: Jacobus Cornelius Gideon Kotze Van Der Colf, Johannes Nell, Frances Stander
  • Patent number: 5846510
    Abstract: A process for forming an aqueous chloride leachant from a spent aqueous chloride leach liquor which process comprises passing a spent aqueous chloride leach liquor and gases containing hydrogen chloride through a preconcentrator to form a concentrated aqueous chloride leach liquor by partial evaporation of water therefrom and absorption of hydrogen chloride; withdrawing a portion of the concentrated aqueous chloride leach liquor; roasting the remainder of the concentrated aqueous chloride leach liquor to generate a metal oxide, and gases containing hydrogen chloride; and passing the gases containing hydrogen chloride to the preconcentrator.
    Type: Grant
    Filed: July 15, 1997
    Date of Patent: December 8, 1998
    Assignee: Technological Resources Pty Ltd
    Inventors: Michael John Hollitt, Ross Alexander McClelland
  • Patent number: 5730774
    Abstract: A process for removing impurities from a titaniferous material that has been subjected to thermal reduction and which includes a titaniferous phase of general formula M.sub.3 O.sub.5. The thermally reduced titaniferous material is subjected to a secondary heat treatment to covert the M.sub.3 O.sub.5 phase to a more readily leachable M.sub.2 O.sub.3 phase. This material is then cooled and leached in an aqueous acid solution containing hydrochloric acid or sulfuric acid, and the leachate is separated from the titaniferous material to form a purified titaniferous material.
    Type: Grant
    Filed: April 1, 1996
    Date of Patent: March 24, 1998
    Assignee: Technological Resources PTY Ltd.
    Inventors: Michael John Hollitt, Ross Alexander McClelland
  • Patent number: 5660805
    Abstract: A process for beneficiating particulate titanium-bearing ore containing iron oxides is disclosed. The first step of the process entails prereducing the ore to convert about 20-90 percent of the iron oxides in the ore to metallic iron. Next, the prereduced ore is introduced into a mechanical reduction kiln and contacted with HCl and particulate carbonaceous reducing material. The turning and cascading of the materials in the kiln, in the presence of HCl and the reducing material, converts at least some remaining iron oxide in the ore to metallic iron and causes metallic iron to be liberated from the ore grains. Particulate metallic iron having a particle size of at least 50 microns is thereby formed. Finally, the particulate iron is separated from the ore.
    Type: Grant
    Filed: January 26, 1996
    Date of Patent: August 26, 1997
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: James William Reeves, Bo Harry Zander, Aake Sandor Ericson
  • Patent number: 5527469
    Abstract: A titanium oxide hydrolysate slurry prepared by the sulfate process is treated with either an alkali metal hydroxide or an alkali metal carbonate to solubilize the sulfur bound to the titanium at a temperature of from 60.degree. C. to 120.degree. C. and the slurry is treated with an organic acid to remove the alkali metal compounds present. This process produces titanium oxide hydrolysate of high purity.
    Type: Grant
    Filed: June 12, 1995
    Date of Patent: June 18, 1996
    Inventors: Earl R. Lawhorne, Woodford R. Brown, Jr.
  • Patent number: 5489423
    Abstract: In order to efficiently and easily recover a spent sulfuric acid exhasuted, for example, in an acid washing liquid or in producing titanium dioxide by a sulfate method in a large amount, as highly concentrated sulfuric acid, bivalent iron ions in the spent sulfuric acid containing metal sulfate are first oxidized into trivalent iron ions, hydrochloric acid is added to such a liquid and then solvent extraction is carried out.
    Type: Grant
    Filed: October 29, 1992
    Date of Patent: February 6, 1996
    Assignee: Nittetsu Mining Co., Ltd.
    Inventors: Yasuie Mikami, Nobuyoshi Iyatomi
  • Patent number: 5427749
    Abstract: The specification describes a process for producing synthetic rutile from a titaniferous ore or concentrate. The process involves three basic steps which are reduction, removal or iron by leaching or aeration and removal of other impurities by leaching in a solution of a strong mineral acid such as hydrochloric acid or sulphuric acid. The conditions of reduction are controlled to promote the formation of metallic iron, a major rutile phase and a minor impurity bearing phase. The minor impurity phase may be a metatitanate, an anosovite or a pseudobrookite. However, formation of a metatinatate is normally preferred. Suitable reductants include carbonaceous materials or hydrogen bearing gases such as natural gas or synthesis gas. The process is capable of removing more than 80% of each of the contained iron magnesium and manganese remaining as oxides after reduction. Substantial proportions of contained aluminum can also be removed.
    Type: Grant
    Filed: November 2, 1992
    Date of Patent: June 27, 1995
    Assignee: Wimmera Industrial Minerals Pty. Ltd.
    Inventors: Michael J. Hollitt, Brian A. O'Brien, Ian E. Grey
  • Patent number: 5411719
    Abstract: Accordingly the present invention provides a process for producing acid soluble titania which process comprises the steps of:(i) adding a manganese or magnesium compound to a titaniferous mineral if the mineral does not contain sufficient manganese and magnesium to satisfy the following relationship: ##EQU1## where a represents the percentage by weight of MgO contained in the mineral,b represents the percentage by weight of MnO contained in the mineral, andd represents the percentage by weight of TiO.sub.
    Type: Grant
    Filed: September 24, 1993
    Date of Patent: May 2, 1995
    Assignee: Wimmera Industrial Minerals Pty. Ltd.
    Inventors: Michael J. Hollitt, Brian A. O'Brien
  • Patent number: 5409679
    Abstract: The production of titanium dioxide by the sulphate process generates waste substances such as the wash filtrates, which are formed in the washing of titanium dioxide hydrate, and waste gases which contain sulphur dioxide. In this improved process the wash filtrate is used to remove the sulphur dioxide from the waste gas while the sulphuric acid content of the wash filtrate is raised and the sulphuric acid-containing process solution thus obtained is used within the scope of the titanium dioxide production process. The waste gas and the wash filtrate are passed countercurrently through a series of several washing steps and are contacted with each other by introducing the wash liquid into the waste gas in a finely divided form in scrub towers. The sulphuric acid content of the washing fluid is stepwise changed from washing stage to washing stage. The sulphur dioxide content of the waste gas is reduced to values that may be discharged into the ambient atmosphere.
    Type: Grant
    Filed: July 5, 1990
    Date of Patent: April 25, 1995
    Assignee: Kronos, Inc.
    Inventor: Achim Hartmann
  • Patent number: 5271910
    Abstract: A process of treating metal chloride wastes produced by chlorination of titanium ore comprises the steps of:(a) leaching said metal chloride wastes in a hydrochloric acid (HCl)-containing solution to obtain a solution containing solids and dissolved metals,(b) separating said dissolved metals from said solids present in the solution obtained in step (a) to obtain a liquid and a residue,(c) selectively precipitating the metals as their hydroxides by adding a neutralizing agent to the liquid obtained in step (b),(d) separating the precipitate of metal hydroxides obtained in step (c) from the liquid to obtain a residue, and(e) dewatering the residue obtained in step (d).
    Type: Grant
    Filed: March 13, 1990
    Date of Patent: December 21, 1993
    Assignee: Shell Internationale Research Maatschappij B.V.
    Inventors: Andries P. van der Meer, Gerrit van der Lee
  • Patent number: 5248497
    Abstract: This invention provides a process for the recovery of purified ferrous chloride resulting as a by-product during the production of titanium dioxide by the chloride process. The process involves a two-step cooling of a filtered solution containing ferrous chloride and other material in a manner to crystallize the ferrous chloride as a pure product. Such product can then be sold commercially including to companies involved in the waste water treatment business.
    Type: Grant
    Filed: August 7, 1992
    Date of Patent: September 28, 1993
    Assignee: Kronos, Inc.
    Inventors: Achim Hartmann, Erwin Schmeir
  • Patent number: 5186920
    Abstract: The iron content of the TiO.sub.2 -containing precursor is subjected to a direct reduction to effect a metallization of at least 90%. The reduced product is separated into magnetic and nonmagnetic fractions by magnetic separation. To oxidize the metallic iron, the magnetic fraction is subjected to an oxidation in an acid medium with agitation at a pH value below 2, under a pressure of 12 to 24 bars, and at a temperature from 150.degree. to 210.degree. C. with a supply of an oxygen-containing gas that contains at least 90% oxygen. When the suspension has been pressure-relieved, the hematite which has been formed is separated from the TiO.sub.2 concentrate.
    Type: Grant
    Filed: November 19, 1991
    Date of Patent: February 16, 1993
    Assignee: Metallgesellschaft Aktiengesellschaft
    Inventors: Rudolf Heng, Walter Koch, Ali-Naghi Beyzavi
  • Patent number: 5063032
    Abstract: Synthetic rutile is prepared from titaniferous slags containing alkaline-earth metal impurities, such as magnesium oxide, by a method comprising contacting the slag with chlorine at a temperature of at least about 800.degree. C., and then leaching the chlorine-treated slag with hydrochloric acid at a temperature of at least about 140.degree. C.
    Type: Grant
    Filed: March 27, 1990
    Date of Patent: November 5, 1991
    Assignee: QIT-Fer et Titane, Inc.
    Inventor: Michel Gueguin
  • Patent number: 4988495
    Abstract: A process for the preparation of an improved quality TiO.sub.2 pigment by hydrolysis of titanyl sulphate, isolation of the hydrolysis product form the waste acid produced during the hydrolysis, washing of the hydrolysis product and calcination of the hydrolysis product to form the TiO.sub.2 pigment, wherein the hydrolysis of the titanyl sulphate is carried out using separately produced hydrolysis nuclei which have been produced by a reaction of titanium salts with alkaline reagents, and in which waste acid and/or wash liquid containing waste acid is added after at least 50% of the total duration of the hydrolysis process.
    Type: Grant
    Filed: December 15, 1989
    Date of Patent: January 29, 1991
    Assignee: Bayer Aktiengesellschaft
    Inventors: Gerhard Wiederhoft, Eckhard Bayer, Wolfgang D. Muller, Gunter Lailach
  • Patent number: 4952387
    Abstract: A process for the separation of metal sulphates from dilute sulphuric acid by evaporative concentration of the sulphuric acid to a concentration of from 55 to 75% by weight H.sub.2 SO.sub.4, cooling of the resulting solution or suspension and mechanically separating the solid metal sulphates and/or hydrogen sulphates, wherein an Fe(III) content of at least 0.01% by weight is ensured before the separation.
    Type: Grant
    Filed: July 13, 1988
    Date of Patent: August 28, 1990
    Assignee: Bayer Aktiengesellschaft
    Inventors: Gunter Lailach, Rudolf Gerken, Wolfgang Rens
  • Patent number: 4933153
    Abstract: A synthetic rutile is prepared from a titaniferous slag, typically containing at least about 1.0 weight percent magnesium oxide and at least some portion of its titanium values as Ti.sub.2 O.sub.3, by a method comprising contacting the slag with chlorine gas at a temperature between about 400.degree. C.-800.degree. C., such that the magnesium oxide and chlorine gas react to form magnesium chloride, and then removing the magnesium chloride from the slag, typically by washing the slag with water. In one embodiment, the synthetic rutile can be further upgraded by subjecting it to either a caustic or acid leaching treatment.
    Type: Grant
    Filed: December 9, 1987
    Date of Patent: June 12, 1990
    Assignee: QIT Fer et Titane, Inc.
    Inventor: Michel Gueguin
  • Patent number: 4917872
    Abstract: A method for producing titanium fluoride comprises: a dissolution process, wherein iron-containing titanium material is dissolved in solutions containing hydrofluoric acid, fluoride solutions being produced; a first crystallization and separation process, wherein ferric fluoride is crystallized and ferric fluoride crystals thus obtained are separated from the fluoride solutions by cooling the fluoride solutions, crude titanium fluoride solutions being produced; a second crystallization and separation process, wherein a mixed salt of (NH.sub.4).sub.2 TiF.sub.6 and (NH).sub.3 FeF.sub.6 is crystallized and separated by mixing ammonium fluoride solutions with the crude titanium fluoride solutions to obtain a mixture and concentrating the mixture; a first pyrolysis process, wherein the ammonium fluoride salt is pyrolyzed at a temperature of from 300.degree. to 800.degree. C. in a stream of dry gas after having dried the ammonium fluoride, solid ferric fluoride (FeF.sub.3) and gaseous TF.sub.4, HF and NH.sub.
    Type: Grant
    Filed: November 25, 1988
    Date of Patent: April 17, 1990
    Assignee: NKK Corporation
    Inventors: Keisuke Nakahara, Hideyuki Yoshikoshi, Toshio Hinami, Takaho Kawawa
  • Patent number: 4891206
    Abstract: A process for the extensive removal of undesirable metal ions, particularly vanadium ions, in the course of the concentration of dilute iron(II) sulfate-containing sulfuric acid solutions. The sulfuric acid solutions are concentrated by the evaporation of water and the separation of iron(II) sulfate to a content of 60 to 70% by weight H.sub.2 SO.sub.4. According to the invention, the content of trivalent titanium in the solution is adjusted such that the content of trivalent iron does not exceed 0.1 g/l. The trivalent titanium may be added from the outside, if not already present in an adequate amount in the solution, or may be formed in situ from the tetravalent titanium present in the solution by the addition of a reducing agent. Prior to the final concentration, part of the iron may be precipitated and separated as iron(II) sulfate heptahydrate by means of preconcentration and cooling of the preconcentrated sulfuric acid solution.
    Type: Grant
    Filed: August 17, 1984
    Date of Patent: January 2, 1990
    Assignee: Kronos Titan, GmbH
    Inventors: Achim M. Kulling, Helmut Steinhausen
  • Patent number: 4416693
    Abstract: Titanium metal values may be recovered from a metal-bearing source containing titanium and iron by subjecting the source to an oxidation treatment and a reductive roast. After having crushed the source to a desired particle size, the reduced source is then leached by treatment with a halogen-containing compound to form soluble halides, following which the soluble titanium halide is precipitated as titanium dioxide by treatment with an iron oxide such as ferric oxide and recovered. The amount of titanium dioxide which is recovered may be optimized by utilizing a reductant such as hydrogen or carbon monoxide in an amount in the range of from about 1.5 to about 4.5 times the stoichiometric amount required to reduce the iron oxide to metallic oxide during the reductive roast.
    Type: Grant
    Filed: December 17, 1981
    Date of Patent: November 22, 1983
    Assignee: UOP, Inc.
    Inventor: William K. Tolley
  • Patent number: 4390365
    Abstract: The instant invention relates to a process for the preparation of titanium metal from an ore comprising titanium oxides which process comprises the steps of fluorinating the ore to convert the titanium oxides to titanium fluorides and then reducing the titanium fluorides to the metal. Such reduction may be carried out by contacting the titanium fluorides as a molten salt mixture with a molten alloy of zinc and aluminum at conditions whereby titanium is converted into a titanium-zinc alloy and the aluminum is converted into fluorides of aluminum. The titanium zinc alloy is separated from the fluorides of aluminum and the zinc is distilled from the alloy to leave behind titanium sponge. The ore may be an ilmenite ore and the fluorination may be carried out by contacting said ilmenite ore with a fluosilicate salt such as sodium fluosilicate.
    Type: Grant
    Filed: December 15, 1980
    Date of Patent: June 28, 1983
    Assignee: Occidental Research Corporation
    Inventors: Robert A. Hard, Martin A. Prieto
  • Patent number: 4384883
    Abstract: A reduction process for the metallization of ferrotitaniferous materials comprising a partial metallization at a low temperature with hydrogen followed by a high temperature reduction with a carbonaceous reductant.
    Type: Grant
    Filed: March 31, 1982
    Date of Patent: May 24, 1983
    Assignee: ICI Australia Limited
    Inventor: Donald J. Fensom
  • Patent number: 4304758
    Abstract: A process for the preparation of a hydrolyzable titanyl sulphate solution comprising adding sulphuric acid having a concentration greater than about 86% to a ternary mixture of two slags and an ilmenite to bring the proportion by weight of H.sub.2 SO.sub.4 to TiO.sub.2 to from about 1.7:1 to 2.2:1 and adding water, dilute sulphuric acid or oleum in amount sufficient to bring the H.sub.2 SO.sub.4 concentration to from about 86 to 96%, thereby to form the titanyl sulphate solution, the first slag having a TiO.sub.2 content greater than about 80% and a Ti(III) content of about 22 to 40%, the second slag having a TiO.sub.2 content of about 60 to 80% and a Ti(III) content of about 5 to 15%, and the ilmenite having a ratio of Fe(III) to Fe(II) of from about 1:1 to 10:1, the slags and ilmenite being present in such proportions that the ternary mixture of raw materials obtained has a molar ratio of Ti(III) to Fe(III).gtoreq.1.4.
    Type: Grant
    Filed: December 5, 1980
    Date of Patent: December 8, 1981
    Assignee: Bayer Aktiengesellschaft
    Inventors: Hilmar Rieck, Walter Gutsche, Peter Woditsch, Peter Panek
  • Patent number: 4288415
    Abstract: A process is provided for the manufacture of titanium compounds and particularly titanium dioxide wherein excess titaniferous bearing material is reacted with dilute sulfuric acid having a concentration of between about 25% and about 60% by weight at a temperature below about 140.degree. C., and in the presence of a reducing agent which affects the reduction of ferric iron to ferrous iron. Thereafter, the titanium sulfate may be recovered or further processed to provide titanium dioxide hydrate accompanied by recycling the spent acid for reaction with the titaniferous bearing material charged to the process. The titanium hydrate may be calcined to provide titanium dioxide.
    Type: Grant
    Filed: May 30, 1980
    Date of Patent: September 8, 1981
    Assignee: NL Industries, Inc.
    Inventors: Joseph A. Rahm, Donald G. Cole
  • Patent number: 4288416
    Abstract: A process is provided for the manufacture of titanium compounds and particularly titanium dioxide wherein excess titaniferous bearing material is reacted with dilute sulfuric acid having a concentration of between about 25% and about 60% by weight at a temperature below about 140.degree. C. Thereafter, the titanium sulphate may be recovered or processed to provide titanium dioxide hydrate accompanied by recycling the spent acid for reaction with the titaniferous bearing material charged to the process. The titanium hydrate may be calcined to provide titanium dioxide pigment.
    Type: Grant
    Filed: May 30, 1980
    Date of Patent: September 8, 1981
    Assignee: NL Industries, Inc.
    Inventors: Brian R. Davis, Joseph A. Rahm
  • Patent number: 4288417
    Abstract: A process is provided for the manufacture of titanium dioxide pigment wherein excess ilmenite ore is reacted with dilute sulfuric acid having a concentration of between about 25% and about 60% by weight in the presence of an iron reductant, and in preferably at least two stages wherein the first stage is maintained at a temperature up to about 140.degree. C. and the second stage is conducted at a lower temperature (than the first stage) which is below about 100.degree. C. to provide a salt solution of titanium and iron. Thereafter, the titanium is hydrolyzed to provide titanium dioxide hydrate accompanied by recycling the spent acid from the hydrolysis for reaction with the ilmenite ore charged to the process. The titanium hydrate is calcined to provide titanium dioxide pigment.
    Type: Grant
    Filed: October 29, 1980
    Date of Patent: September 8, 1981
    Assignee: NL Industries, Inc.
    Inventors: Joseph A. Rahm, Donald G. Cole
  • Patent number: 4288418
    Abstract: A process is provided for the manufacture of titanium dioxide pigment wherein excess ilmenite ore is reacted with dilute sulfuric acid having a concentration of between about 25% and about 60% by weight and in preferably at least two stages wherein the first stage is maintained at a temperature up to about 140.degree. C. and the second stage is conducted at a lower temperature (than the first stage) which is below about 100.degree. C. to provide a salt solution of titanium and iron. Thereafter, the titanium is hydrolyzed to provide titanium dioxide hydrate accompanied by recycling the spent acid from the hydrolysis for reaction with the ilmenite ore charged to the process. The titanium hydrate is calcined to provide titanium dioxide pigment.
    Type: Grant
    Filed: October 29, 1980
    Date of Patent: September 8, 1981
    Assignee: NL Industries, Inc.
    Inventors: Brian R. Davis, Joseph A. Rahm
  • Patent number: 4275041
    Abstract: A process is provided for the manufacture of a stable titanyl sulfate solution by diluting a reaction mixture containing iron sulfate and titanyl sulfate with a material selected from water, a titanyl sulfate solution, and mixtures thereof. The titanyl sulfate solution may be recovered or processed to provide titanium dioxide hydrate which may be calcined to provide titanium dioxide pigment.
    Type: Grant
    Filed: September 19, 1980
    Date of Patent: June 23, 1981
    Assignee: NL Industries, Inc.
    Inventors: Joseph L. Waldman, Edgar Klein, Achim Kulling, Joseph A. Rahm
  • Patent number: 4202863
    Abstract: In a process for recovering titanium metal values from a titanium bearing source which also contains iron, the source is subjected to a reductive roast followed by a leach of the reduced source with hydrogen chloride. The suppression of the dissolution of titanium during the leaching step of the process will be effected by the addition of a phosphoric acid to the leaching solution.
    Type: Grant
    Filed: November 27, 1978
    Date of Patent: May 13, 1980
    Assignee: UOP Inc.
    Inventor: William K. Tolley
  • Patent number: 4199552
    Abstract: An improved process for the production of synthetic rutile from ore containing titanium and iron, such as ilmenite ore, by a multi-step procedure employing controlled reduction, controlled oxidation and acid leaching. More specifically, the ilmenite ore first is reduced thermally such that substantially all of the iron (III) present has been converted to iron (II) and some metallic iron. The reduced ore then is oxidized with an oxidizing gas substantially free of elemental oxygen to convert the metallic iron to iron (II) without the substantial formation of iron (III). The oxidized ore then is leached to remove the iron (II) and calcined to produce synthetic rutile. The synthetic rutile so produced contains in excess of 92 percent titanium dioxide and less than 2 percent iron (III), by weight. Often, the synthetic rutile contains less than 1 percent total iron by weight.
    Type: Grant
    Filed: May 26, 1978
    Date of Patent: April 22, 1980
    Assignee: Kerr-McGee Corporation
    Inventor: Theodore A. Rado
  • Patent number: 4183899
    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.
    Type: Grant
    Filed: March 10, 1978
    Date of Patent: January 15, 1980
    Assignee: SCM Corporation
    Inventor: James P. Bonsack