Treating With Sulfur Or Halogen Containing Acid Patents (Class 423/82)
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Patent number: 6803024Abstract: This invention relates to a method of treating titania slag to increase the leachability of impurities from the slag consisting of the steps of sizing the titania slag to a particle size from 75 to 850 &mgr;m; oxidizing the sized slag particles at a temperature from about 700° C. to below about 900° C. causing the iron present in the slag to concentrate at the exposed surfaces of the slag particles and/or causing an anatase phase to stabilize in the slag, causing a major portion of the iron in the Fe(II) state to convert to the Fe(III) state, and causing the titanium in the Ti(III) state to be converted to the Ti(IV) state; and reducing the oxidized slag in a reducing atmosphere from about 700° C. to about 950° C. to convert a major portion of the iron in the Fe(III) state to the Fe(II) state. The invention also relates to a method of beneficiating titania slag to increase the TiO2 content thereof wherein the above treated slag is leached with acid.Type: GrantFiled: June 15, 2001Date of Patent: October 12, 2004Assignee: Ipcor NVInventors: Jacobus Philippus Van Dyk, Nanne Mattheus Vegter, Cornelia Petronella Visser, Thomas De Lange, John David Winter, Ernest Alan Walpole, Johannes Nell
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Patent number: 6780384Abstract: A method of recovering zirconium values from an ore containing zircon, baddeleyite, and uranium is disclosed. The method includes fusing the ore with soda ash and contacting the resulting fused ore with sulfuric acid, which generates an acid leach liquor that contains zirconium and uranium values and solids that comprise baddeleyite and silica. Baddeleyite is recovered by contacting it with sulfuric acid to convert baddeleyite to zirconium sulfate, which can be dissolved in the acid leach liquor. The method also includes separating zirconium from uranium by solvent extraction followed by precipitation.Type: GrantFiled: March 7, 2002Date of Patent: August 24, 2004Assignee: Cotter Corporation (NSL)Inventors: Allen L. Williams, Robert W. Philips, Jr., David R. Tierney, Daniel R. Dilday
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Patent number: 6699446Abstract: A method for the production of titanium metal from titanium-bearing ore. The method comprises leaching said ore or a concentrate thereof with an aqueous solution of a hydrogen halide; separating solids from the leach solution, to provide a leachate solution. The leachate solution may be subjected to extraction with an immiscible organic phase to selectively remove iron values to provide high purity iron products. Titanium may be separated from raffinate as TiO2 or solvent extract and thermal stripping. TiO2 may also be separated in the initial leach solution. Preferably, the titanium halide is titanium tetrachloride.Type: GrantFiled: January 25, 2001Date of Patent: March 2, 2004Inventors: Vaikuntam Iyer Lakshmanan, Ramamritham Sridhar, Marc Murray Rishea, Robert Joseph de Laat
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Patent number: 6627165Abstract: A process for upgrading of titaniferous material containing silica, including pretreating the titaniferous material by alkaline leaching to precipitate the silica as an aluminosilicate which is amenable to further leaching. Subsequently, the pretreated titaniferous material is leached under acid conditions, causing the silica to enter solution under conditions such that the silica is not hydrolysed or precipitated as a silicate.Type: GrantFiled: June 28, 2001Date of Patent: September 30, 2003Assignee: Technological Resources PTY LTDInventors: Ross Alexander McClelland, Michael John Hollitt
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Patent number: 6500396Abstract: A method for the production of titanium metal from titanium-bearing ore. The method comprises leaching said ore or a concentrate thereof with an aqueous solution of a hydrogen halide; separating solids from the leach solution, to provide a leachate solution. The leachate solution may be subjected to extraction with an immiscible organic phase. Titanium halide is separated from the organic phase by stripping. Preferably, the titanium halide is titanium tetrachloride.Type: GrantFiled: November 17, 1999Date of Patent: December 31, 2002Inventors: Vaikuntam Iyer Lakshmanan, Ramamritham Sridhar, Marc Murray Rishea, Robert Joseph de Laat
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Publication number: 20020168310Abstract: An industrially realistic process for upgrading of titaniferous materials is disclosed. The process comprises the following steps: (i) a pretreatment which has the effect of rendering silica amenable to leaching under the particular conditions of a subsequent leach, and (ii) an aqueous leach in the presence of an acid, the conditions of which are chosen such that silica which enters solution is not hydrolysed or precipitated as a silicate. The pretreatment step (i) may comprise alkaline leaching, roasting or smelting. The leaching step (ii) may be conducted at low solids densities.Type: ApplicationFiled: June 28, 2001Publication date: November 14, 2002Inventors: Ross A. McClelland, Michael J. Hollitt
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Patent number: 6471743Abstract: Disclosed and claimed are efficient methods for leaching minerals from ores using an acidic solution such as sulfuric acid. Additional factors which can improve mineral recovery include the use of an alkali metal halide, grinding the ore, addition of a carbon source, and/or, adjustment of the temperature at which the process is carried out. Minerals such as titanium, iron, nickel, cobalt, silver and gold may be recovered by the methods of the present invention.Type: GrantFiled: February 18, 2000Date of Patent: October 29, 2002Assignee: MBX Systems, Inc.Inventors: Tom L. Young, Michael G. Greene, Dennis R. Rice, Kelly L. Karlage, Sean P. Premeau
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Patent number: 6468483Abstract: 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: GrantFiled: May 3, 2001Date of Patent: October 22, 2002Assignee: Goldendale Aluminum CompanyInventors: Robert J. Barnett, Michael B. Mezner
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Patent number: 6447738Abstract: 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: GrantFiled: August 24, 2000Date of Patent: September 10, 2002Assignee: Solv-Ex CorporationInventors: John S. Rendall, Massoud Ahghar, Jerry V. Fox, Fred A. Aiken
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Patent number: 6423291Abstract: The invention provides a process for the production of titanium tetrachloride (TiCl4) by the chlorination of titanium values in a titanium-containing starting material. The process includes exposing the starting material to a chlorinating agent and contacting the starting material with an inert liquid while the starting material is exposed to the chlorinating agent. The inert liquid is at a temperature of 200-350° C. and is at a pressure of 5-100 atmospheres (1 atmosphere=101.325 kN/m2). This causes the starting material to react with the chlorinating agent to form TiCl4. The invention also extends to TiCl4 whenever made in accordance with the method.Type: GrantFiled: August 10, 2000Date of Patent: July 23, 2002Inventors: Andrew Kenneth Stone, David Steyn Van Vuuren, Kevin Frans Pieter Cilliers
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Patent number: 6346223Abstract: A process for the production of titanium concentrates from anatase ores with high utilization of the iron contents of the raw ore involving the steps of calcining mechanically treated ore in the presence of an alkali metal carbonate followed by dilute leachings in both alkaline and acid media. No reducing agents are employed during calcination, avoiding the iron contents of the ore to be solubilized in the leaching steps. The final concentrate, which is rich in titanium and iron and has a low content of impurities, can be used as a raw material for the production of titanium slag.Type: GrantFiled: October 19, 1998Date of Patent: February 12, 2002Assignee: Companhia Vale Do Rio DoceInventors: Marcelo De Matos, Lino Rodrigues De Freitas, Ronaldo De Moreira Horta
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Patent number: 6306195Abstract: The present invention relates to an improved process for the preparation of high grade synthetic rutile from ilmenite with pig iron as a by-product. The process comprises subjecting ilmenite to reduction with coal, cooling and removing unreacted coal to obtain a product having 80-95% metallization, smelting the metallized ilmenite mixed with less than 10% carbon (w/w) in a transferred arc plasma using arc current, under flow of inert gas for a fixed time. The metal is then separated as pig iron and TiO2 as slag, the slag ground followed by oxidation at high temperature in the presence of an oxidizing gas, the oxidized product being leached with dilute HCl followed by filtration, washing and drying to obtain synthetic rutile.Type: GrantFiled: March 24, 2000Date of Patent: October 23, 2001Assignee: Council of Scientific and Industiral ResearchInventors: Pawvathu Narayanan Nair Mohan Das, Karval Harikrishna Bhat, Melay Eriyat Kochu Janaki, Sreedharan Sasibhushanan, Parthasarathi Mukherjee, Bishnu Charan Rabindha Mohanty, Hem Shanker Ray
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Publication number: 20010016182Abstract: The present invention is a process for controlling, at an aim point, the passivation of aluminum chloride in the chlorinator discharge stream in a process for making titanium tetrachloride.Type: ApplicationFiled: December 18, 2000Publication date: August 23, 2001Inventors: James Timothy Cronin, Thomas Shields Elkins, Hans Hellmut Glaeser, Lisa Edith Helberg, Angela Ruth Strzelecki
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Patent number: 6248302Abstract: 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: GrantFiled: February 4, 2000Date of Patent: June 19, 2001Assignee: Goldendale Aluminum CompanyInventors: Robert J. Barnett, Michael B. Mezner
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Patent number: 6090354Abstract: A process for production of titanium oxide comprises digesting an ilmenite ore in which at least 92% by weight of the iron which is present is in the ferrous form, if necessary adding a reducing agent and subsequently precipitating hydrous titanium oxide. When a reducing agent is added the amount used is equivalent to less than 4.0% by weight metallic iron calculated with respect to ilmenite ore. The process enables an increased throughput on a pigment plant and less co-product in the form of iron compounds is produced.Type: GrantFiled: March 24, 1997Date of Patent: July 18, 2000Assignee: Tioxide Group Services LimitedInventors: John Henry Russell, David Ian Rochester, Kenneth Burns, Roger Philip Bacon
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Patent number: 6048505Abstract: A non-polluting liquid-phase process and a supporting system of apparatus for producing titanium dioxide from titanium ore or slag provide a more economical sulfate process for preparing anatase. The ore or slag is reacted with hot sulfuric acid. The reaction product is filtered and washed before being combined with acid water, in which the solids are partially dissolved. The resulting suspension is filtered, and the filtrate hydrolyzed to convert titanium values therein to titanium dioxide hydrate, which is calcined to produce anatase pigment.Type: GrantFiled: August 22, 1997Date of Patent: April 11, 2000Assignee: Kemicraft Overseas LimitedInventors: Jorge Miller, Brian Richard Davis, Joseph Aloysius Rahm, Eric James Madsen
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Patent number: 5958355Abstract: A process for reacting a zirconia-based material comprises reacting, in a reaction step, plasma dissociated zircon with aqueous hydrogen fluoride to produce a soluble fluoro zirconic acid compound.Type: GrantFiled: June 2, 1997Date of Patent: September 28, 1999Assignee: Atomic Energy Corporation of South Africa LimitedInventor: Johannes Theodorus Nel
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Patent number: 5866750Abstract: A method for recovering titanium and vanadium compounds, such as alkoxides, from a liquid hydrocarbon mixture by hydrolyzing the mixture with a base or acid wash having a sufficiently different density so that two liquid phases form, and separating the two liquid phases.Type: GrantFiled: November 1, 1995Date of Patent: February 2, 1999Assignee: Union Carbide Chemicals & Plastics Technology CorporationInventors: Robert Stephen Tomaskovic, Michael Wayne Potter, William Charles Malven
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Patent number: 5863514Abstract: Titanium oxide, comprising lamina shaped titanium oxide particles having a thickness of 10-30 nm and a width of 0.5 to 1 .mu.m, may be prepared by exfoliating a layered titanic acid powder having a formula H.sub.x Ti.sub.2-x/4 O.sub.4.nH.sub.2 O, where x=0.60-0.75, to form a titania sol; followed by drying and heating, to obtain a titanium oxide. The layered titanic acid powder may be prepared by contacting cesium titanate having an orthorhombic layered structure with an aqueous acid solution.Type: GrantFiled: January 30, 1996Date of Patent: January 26, 1999Assignee: National Institute for Research in Inorganic MaterialsInventors: Takayoshi Sasaki, Mamoru Watanabe, Masayuki Tsutsumi
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Patent number: 5830420Abstract: A method is disclosed including: (a) sizing a titania slag to a particle size range of from 75 microns to 850 microns; (b) oxidizing the sized titania slag by contacting the sized titania slag with an oxygen containing gas at a temperature of at least about 950.degree. C. for a period of at least about 20 minutes such that a substantial portion of the iron oxide is converted to a ferric state, such that the reduced titanium oxides are converted to a tetravalent state, and such that at least a major portion of the glassy silicate phase is decomposed; (c) reducing the oxidized titania slag in a reducing atmosphere at a temperature of at least about 700.degree. C. for a period of at least about 30 minutes such that the ferric state iron oxide is converted to a ferrous state; (d) leaching the reduced titania slag with mineral acid at a temperature of at least 125.degree. C.Type: GrantFiled: November 21, 1995Date of Patent: November 3, 1998Assignee: QIT-Fer et Titane Inc.Inventors: Krzysztof Borowiec, Alfonso E. Grau, Michel Gueguin, Jean-Fran.cedilla.ois Turgeon
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Patent number: 5826162Abstract: A process for facilitating removal of one or more impurities from titaniferous material containing the impurities in a form which is highly soluble in acid. The material is in turn leached with a sulphuric acid solution and with a hydrochloric acid solution in either order. To enhance the susceptibility of the impurities to removal, the hydrochloric acid leach is augmented by one or more of the following: (i) addition of an effective amount of an added chloride salt; (ii) pre-treatment of the titaniferous material with a solution of an effective amount of a carbonate salt, preferably an alkali metal or alkaline earth metal carbonate; and/or (iii) pre-treatment of the titaniferous material with a solution of an effective amount of a hydroxide, preferably an alkali metal or alkaline earth metal hydroxide.Type: GrantFiled: October 28, 1996Date of Patent: October 20, 1998Assignee: RGC Mineral Sands LimitedInventors: Halil Aral, Warren John Bruckard, David Edward Freeman, Ian Edward Grey, Martin Richard Houchin, Kenneth John McDonald, Graham Jeffrey Sparrow, Kaye Patricia Hart, Harold Robert Harris
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Patent number: 5688477Abstract: A process for treating dissociated zircon comprises reacting dissociated zircon with gaseous hydrogen fluoride at an elevated reaction temperature. The reaction temperature is controlled to obtain at least one desired zirconium-based compound and at least one desired silicon-based compound.Type: GrantFiled: January 24, 1995Date of Patent: November 18, 1997Assignee: Atomic Energy Corporation of South Africa LimitedInventor: Jonathan Nel
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Patent number: 5597515Abstract: A process for producing a conductive, fluorine-doped titanium dioxide product which is doped throughout, said process comprising the steps of: (a) reacting the precursors in a system to form fluorine-doped TiO.sub.2, said precursors consisting essentially of a titanium alkoxide and a fluorine source; (b) reducing the fluorine-doped titanium dioxide product at a temperature sufficient to form said conductive, fluorine-doped titanium dioxide product; and (c) recovering the reduced product.Type: GrantFiled: September 27, 1995Date of Patent: January 28, 1997Assignee: Kerr-McGee CorporationInventors: James W. Kauffman, Bruce R. Palmer
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Patent number: 5527469Abstract: 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: GrantFiled: June 12, 1995Date of Patent: June 18, 1996Inventors: Earl R. Lawhorne, Woodford R. Brown, Jr.
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Patent number: 5470550Abstract: Zirconium containing less than about 400 ppm aluminum/zirconium is produced by precipitating zirconium sulfate from an aqueous stream containing from 0.5 M to 2 M zirconium oxychloride and contaminated with from 1000 to 3000 ppm aluminum/zirconium and having an acidity of greater than 1.5 N total acid per M zirconium. Ammonium hydroxide having a concentration of at least 14% by weight is added to the zirconium-containing solution to adjust the acidity to between 0.6 and 1.2 N total acid/M zirconium. Because the acidity adjustment results in the premature and undesired precipitation of zirconium hydroxide and aluminum hydroxide, the solution is maintained at a temperature of 60.degree. C. or more for 15 minutes to 60 minutes to dissolve at least some of the zirconium hydroxide without permitting the undissolved zirconium hydroxide to dehydrate to the extent that a gelatinous zirconium oxide precipitate forms. Ammonium sulfate or sulfuric acid is then added to the acid adjusted solution to provide a 0.6 to 0.Type: GrantFiled: December 30, 1993Date of Patent: November 28, 1995Assignee: Westinghouse Electric CorporationInventor: Donald O. Voit
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Patent number: 5468463Abstract: A process for the preparation of very pure titanium dioxide by reacting titanium tetrahalides with sulphuric acid, hydrolysis the titanyl sulphate solution obtained and calcining the hydrolysate is disclosed wherein the reaction between titanium tetrahalide and aqueous 20-40% by weight strength sulphuric acid is performed in such a way that crystallisation of titanyl sulphate does not take place, the hydrogen halide is separated, the solution is optionally concentrated and filtered and then the ratio by weight of sulphuric acid to titanium dioxide is adjusted to between 1.7 and 2.0 and the titanium dioxide concentration is adjusted to between 250 and 300 g/l, the solution is hydrolyzed and the resulting titanium oxide hydrate is filtered off and calcined to give Futile or anatase.Type: GrantFiled: July 29, 1994Date of Patent: November 21, 1995Assignee: Bayer AktiengesellschaftInventors: Kai Butje, Jurgen Kischkewitz
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Patent number: 5409679Abstract: 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: GrantFiled: July 5, 1990Date of Patent: April 25, 1995Assignee: Kronos, Inc.Inventor: Achim Hartmann
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Patent number: 5397554Abstract: Hydrolyzing finely divided, solid Group IVB metal chlorides by gradually introducing the finely divided solids into the mixing zone of a high intensity mixer operating on an aqueous solution produces solid Group IVB metal oxy salts such as ZrOCl.sub.2.8H.sub.2 O.Type: GrantFiled: February 15, 1994Date of Patent: March 14, 1995Assignee: Westinghouse Electric CorporationInventor: Donald O. Voit
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Patent number: 5298169Abstract: Disclosed is a process for treating waste sulfuric acid generated from a process for producing titanium dioxide pigment by treating titanium slag with sulfuric acid. The waste acid is treated in a first step with a calcium-containing material to produce a gypsum suspension which is filtered and from which a filtrate is recovered. The filtrate is treated in a second step with a calcium-containing substance and clarification solids from the treatment of the titanium slag with sulfuric acid. A precipitate is produced in this second step which is subsequently filtered. The precipitate is suitable for disposal in a landfill.Type: GrantFiled: August 21, 1992Date of Patent: March 29, 1994Assignee: Kronos, Inc.Inventors: Roger Laferriere, Pierre Beaupre
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Patent number: 5271910Abstract: 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: GrantFiled: March 13, 1990Date of Patent: December 21, 1993Assignee: Shell Internationale Research Maatschappij B.V.Inventors: Andries P. van der Meer, Gerrit van der Lee
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Patent number: 5229087Abstract: A process for the preparation of titanium dioxide by the sulphate process in which titanium raw materials are decomposed with sulphuric acid, the resulting titanyl sulphate is hydrolyzed, the waste acid is separated from the hydrolyzate and evaporated to a concentration of 60 to 70%, sulphuric acid is separated from the solid metal sulphates, and the sulphuric acid which has been concentrated by evaporation is used again for the decomposition of the titanium raw material, the improvement wherein the 60 to 70% sulphuric acid is concentrated to 70 to 80% H.sub.2 SO.sub.4 in a further evaporation stage and the concentration of a part of this sulphuric acid is raised to a concentration of 98 to 99% H.sub.2 SO.sub.4 by the absorption of SO.sub.3 and then used together with the remainder of the above-mentioned 70 to 80% sulphuric acid for the decomposition of titanium raw materials.Type: GrantFiled: May 14, 1990Date of Patent: July 20, 1993Assignee: Bayer AktiengesellschaftInventors: Karl-Heinz Schultz, Gunter Lailach, Rudolf Gerken
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Patent number: 5186920Abstract: 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: GrantFiled: November 19, 1991Date of Patent: February 16, 1993Assignee: Metallgesellschaft AktiengesellschaftInventors: Rudolf Heng, Walter Koch, Ali-Naghi Beyzavi
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Patent number: 5169619Abstract: There is provided a method of producing titanium oxides which comprises: admixing an aqueous solution of titanium tetrachloride with sulfuric acid in a molar ratio of sulfuric acid to titanium tetrachloride of at least 0.5 adding an alklai to the resultant solution to produce titanium hydroxide; and drying and calcining the titanium hydroxide. A further method is provided which comprises: adding a solution of an alkali to an aqueous solution of titanium tetrachloride having a concentration of not more than 2.5 moles/l at temperatures of not less than 50.degree. C., thereby to substantially thermally hydrolyze the titanium tetrachloride and to produce titanium hydroxide; and drying and calcining the titanium hydroxide.Type: GrantFiled: February 12, 1991Date of Patent: December 8, 1992Assignee: Sakai Chemical Industry Co., Ltd.Inventors: Masafumi Yoshimoto, Tadao Nakatsuji, Kazuhiko Nagano
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Patent number: 5094834Abstract: In the production of TiO.sub.2 pigments by the steps of digesting titanium-containing raw materials with sulfuric acid, hydrolyzing the titanyl sulfate obtained, separating the waste acid from the hydrolyzate, bleaching the hydrolyzate and calcining the hydrolyzate after addition of rutilizing nuclei and standardizing chemicals to form TiO.sub.2 pigments, and recovering sulfuric acid from the waste acid, the improvement which comprises employing as the rutilizing nuclei nuclei produced from part of the bleached and then washed hydrolyzate, which nuclei are added to the remainder of the bleached and washed hydrolyzate before calcination.Type: GrantFiled: October 31, 1990Date of Patent: March 10, 1992Assignee: Bayer AktiengesellschaftInventors: Gerhard Wiederhoft, Gunter Lailach
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Patent number: 5085837Abstract: Process for purifying TiO.sub.2 ore consisting essentially of subjecting the ore to two or more leaching treatments, said leaching treatments alternating between use of an aqueous solution of a mineral acid and an aqueous solution of an alkali metal compound selected from the group consisting essentially of alkali metal carbonates, hydroxides or mixtures thereof.Type: GrantFiled: December 27, 1990Date of Patent: February 4, 1992Assignee: E. I. Du Pont de Nemours and CompanyInventors: Tze Chao, George H. Senkler, Jr.
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Patent number: 5068093Abstract: Titanium slag and ilmenite are subjected to a parallel treatment with sulphuric acid obtained by mixing different proportions of sulphuric acid having concentrations of about 98.5% by weight and about 85% by weight, respectively. The reaction mixtures have a temperature slightly below a predetermined starting temperature and the reactions are started by adding small quantities of superheated steam having a temperature above the predetermined starting temperature. The thus obtained solutions are separated from the respective treatment residues and combined. The combined solutions are further processed for obtaining titanium dioxide. The mother liquor constitutes sulphuric acid of a concentration in the range of about 23% by weight and containing metal sulphates. This mother liquor is concentrated to a sulphuric acid concentration of approximately 85% by weight and recycled.Type: GrantFiled: November 17, 1988Date of Patent: November 26, 1991Assignee: Sulzer-Escher Wyss AGInventor: Josef Mauer
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Patent number: 5063032Abstract: 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: GrantFiled: March 27, 1990Date of Patent: November 5, 1991Assignee: QIT-Fer et Titane, Inc.Inventor: Michel Gueguin
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Patent number: 5053144Abstract: The method of the invention is advantageously applicable to realize a multistage chemical process during which liquid clarifiers suitable for the purification of water and sewage, furthermore, fine-disperse pulverulent solid products utilizable as pait pigments and fillers may be recovered. Each final product of the multistage chemical processes is a useful material, so the whole technology is waste free.Type: GrantFiled: April 2, 1990Date of Patent: October 1, 1991Assignee: Aquatech KernyezeteedelmiInventors: Endre Szirmai, Sandor Babusek, Gezz Balogh, Atilla Nedves, Gyula Horvath, Zoltan Lebenyi, James Pinter
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Patent number: 5011666Abstract: Process for purifying TiO.sub.2 ore consisting essentially of subjecting the ore to two or more leaching treatments, said leaching treatments alternating between use of an aqueous solution of a mineral acid and an aqueous solution of an alkali metal compound selected from the group consisting essentially of alkali metal carbonates, hydroxides or mixtures thereof.Type: GrantFiled: July 28, 1988Date of Patent: April 30, 1991Assignee: E. I. Du Pont de Nemours and CompanyInventors: Tze Chao, George H. Senkler, Jr.
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Patent number: 4988495Abstract: 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: GrantFiled: December 15, 1989Date of Patent: January 29, 1991Assignee: Bayer AktiengesellschaftInventors: Gerhard Wiederhoft, Eckhard Bayer, Wolfgang D. Muller, Gunter Lailach
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Patent number: 4986742Abstract: High-grade titanium dioxide is produced by(a) reacting ilmenite or titanium-containing slag with sulfuric acid,(b) dissolving the material from (a) with water or dilute sulfuric acid,(c) separating insolubles from (b) to obtain a black solution containing titanyl sulfate and foreign metal salts,extracting titanyl sulfate from the black liquor with sulfuric acid and an organic medium containing an organophosphorus compound, separating the foreign metal salts in an aqueous extract phase, recovering titanyl sulfate from the organic extract phase, andhydrolyzing the titanyl sulfate to titanium oxide hydrate.Type: GrantFiled: August 17, 1989Date of Patent: January 22, 1991Assignee: Bayer AktiengesellschaftInventors: Gabriel Denecker, Werner Verhoeven, Joel Leuridan, Domien Sluyts
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Patent number: 4933153Abstract: 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: GrantFiled: December 9, 1987Date of Patent: June 12, 1990Assignee: QIT Fer et Titane, Inc.Inventor: Michel Gueguin
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Patent number: 4902485Abstract: A process for the production of TiO.sub.2 pigments by the sulfate process by digestion of titanium-containing raw materials with sulfuric acid, hydrolysis of the titanyl sulfate formed, purification of the hydrolyzate and calcination of the hydrolyzate in rotary kilns, wherein the calcination conditions are regulated through adjustment of the SO.sub.2 content of the waste gases issuing from the rotary kilns used for calcination.Type: GrantFiled: November 23, 1988Date of Patent: February 20, 1990Assignee: Bayer AktiengesellschaftInventors: Eckhard Bayer, Gunter Lailach
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Patent number: 4863711Abstract: A process for preparing nodular pigmentary titanium dioxide by grinding and mixing a titanium-bearing material, such as sorelslag, with an alkali metal compound such as sodium hydroxide, and roasting the mixture. The roasted material is ground followed by washing and filtering. Thereafter, the solid residue is digested with hydrochloric acid for a time and temperature sufficient to form nodular-shaped solids. After removing the acid by filtration and washing the solid residue, the residue is calcined to provide a nodular titanium dioxide pigment.Type: GrantFiled: September 29, 1987Date of Patent: September 5, 1989Assignee: The Dow Chemical CompanyInventor: Henrik R. Heikel
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Patent number: 4822575Abstract: The invention concerns processes for the preparation of zirconium compositions which on calcination form zirconia. The zirconium compositions are prepared by the addition of an ammonia source to an aqueous zirconium sulfate solution to give a solution pH in the range of from 0.1 to 2.5 and preferably 1.0 to 2.0. The zirconium composition precipitated from solution appears crystalline, is readily collected by filtration and has low levels of metallic impurities. Therefore, the process of the invention may be used to advantage in the purification zirconium compounds.The invention also includes the zirconium compositions and processes for the purification of zirconium compounds including zirconia.Type: GrantFiled: January 2, 1987Date of Patent: April 18, 1989Assignee: ICI Australia LimitedInventors: Kian F. Ngian, Angus J. Hartshorn, David H. Jenkins
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Patent number: 4810682Abstract: A process for production of useful materials including a product of similar composition to nepheline involves contacting a slurry of red mud with sulphur dioxide to dissolve components of the red mud that are soluble in sulphurous acid, removing residual undissolved solids by filtration, and recovering a filtrate containing soda, alumina and silica values, removing free water from the filtrate to produce a crystallized residue, and calcining the crystallized residue.Type: GrantFiled: June 10, 1987Date of Patent: March 7, 1989Assignee: Comalco Aluminum LimitedInventor: William H. Andrews
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Patent number: 4803064Abstract: A process for preparing titanium dioxide in the form of spherical particles having the particle size distribution indicated by dw/dn.ltoreq.2, by hydrolysis of strongly acid solutions of Ti(IV), wherein the molar ratio SO.sub.4.sup.= /Ti(IV) is at least 1.5, and in the presence of cationic polyelectrolytes having a molecular weight higher than 1 million and a ionicity of at least 3 milliequivalents per gram.Type: GrantFiled: September 11, 1987Date of Patent: February 7, 1989Assignee: Montedison S.p.A.Inventors: Franco Montino, Giuseppe Spoto
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Patent number: 4781911Abstract: A titanium dioxide compositon suitable for incorporation into ceramic frit, and process for preparation thereof. A clarified titanium sulfate liquor is hydrolyzed and precipitated to yield relatively large and uniform-sized hydrolysate particles which are easily separated from the acidic liquor by filtration.Type: GrantFiled: April 10, 1987Date of Patent: November 1, 1988Assignee: Kemira, Inc.Inventor: Earl R. Lawhorne
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Patent number: 4780302Abstract: Process for the preparation of alkali metal fluotitanates by fluorination of a titanium ore, reaction with an alkali metal compound, precipitation and separation of the formed alkali metal fluotitanates, wherein the titanium ore is mixed with a hydrofluosilicate solution, the resulting suspension is evaporated at a temperature of 90.degree.-110.degree. C., the residue is subsequently taken up in water or in a mineral acid and the residue solution is neutralized with an alkali metal compound.Type: GrantFiled: June 26, 1986Date of Patent: October 25, 1988Assignee: Stamicarbon B.V.Inventor: Ruud Spijker
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Patent number: 4762552Abstract: The beneficiation or upgrading of an iron-containing titaniferous ore to a synthetic rutile by subjecting the ore to reduction followed by acid leaching of the reduced ore is improved by forming a mixture of the ore and an aqueous sulfuric acid solution, adding a reducing agent to this mixture and then subjecting this mixture containing the reducing agent to reduction at elevated temperatures. The resulting reduced ore, which is characterized by an increase in the ferrous iron content thereof and an increase in its specific surface area, exhibits an enhanced response to subsequent acid leaching to provide a synthetic rutile of improved purity.Type: GrantFiled: June 15, 1987Date of Patent: August 9, 1988Assignee: Kerr-McGee Chemical CorporationInventors: Roger A. Baldwin, William C. Laughlin, Keshav P. Patel, Patricia J. Shreve