Ammoniating Or Sulfating Patents (Class 423/67)
  • Patent number: 8945491
    Abstract: A method for extracting vanadium from shale, the method including: a) grinding the shale into fine powders, mixing the fine powders with an additive in a mass ratio of 1:0.04-0.12 to yield a mixture, heating the mixture to a temperature of between 850 and 950° C. at a heating rate of 5-9° C./min, and baking the mixture for between 30 and 90 min; b) immersing the product in water and acid respectively to yield a first solution and a second solution, combining the two solutions, and performing ion exchange adsorption on the combined solution using a styrene-divinylbenzene based macroporous anion-exchange resin; and c) performing desorption, purification, and precipitation to yield poly ammonium vanadate, and calcining the poly ammonium vanadate at a temperature of between 450 and 530° C. for between 20 and 50 min to yield V2O5.
    Type: Grant
    Filed: August 26, 2013
    Date of Patent: February 3, 2015
    Assignee: Wuhan University of Technology
    Inventors: Yimin Zhang, Xiaobo Zhu, Tao Liu, Jing Huang, Tiejun Chen, Shenxv Bao
  • Publication number: 20140248199
    Abstract: A method for recovering vanadium from a spent slurry catalyst for hydrocarbon oil hydroprocessing is disclosed. In one embodiment after de-oiling, the spent catalyst is treated with ammonia and air, forming a leach slurry. The leach slurry is subsequently treated with a flocculant. After solid-liquid separation to recover the solid residue containing coke and ammonium metavanadate, the solid residue is washed with an ammonium sulfate solution and leached with hot water. After solid-liquid separation to recover a solution containing ammonium metavanadate, the ammonium metavanadate is crystallized and purified from the leach solution.
    Type: Application
    Filed: March 4, 2013
    Publication date: September 4, 2014
    Applicant: Chevron U.S.A. Inc.
    Inventors: Rahul Shankar Bhaduri, Lawrence Paul Zestar
  • Patent number: 8815185
    Abstract: A method for recovering vanadium from a spent slurry catalyst for hydrocarbon oil hydroprocessing is disclosed. In one embodiment after de-oiling, the spent catalyst is treated with ammonia and air, forming a leach slurry. The leach slurry is subsequently treated with a flocculant. After solid-liquid separation to recover the solid residue containing coke and ammonium metavanadate, the solid residue is washed with an ammonium sulfate solution and leached with hot water. After solid-liquid separation to recover a solution containing ammonium metavanadate, the ammonium metavanadate is crystallized and purified from the leach solution.
    Type: Grant
    Filed: March 4, 2013
    Date of Patent: August 26, 2014
    Assignee: Chevron U.S.A. Inc.
    Inventors: Rahul Shankar Bhaduri, Lawrence Paul Zestar
  • Patent number: 8250775
    Abstract: The present invention discloses an automatic plant and a method of stockage in a covered yard of petcoke fuel with high humidity-contents, natural dehumidification up to set humidity values and subsequent reuptake for conveyance to the silos feeding a thermal unit.
    Type: Grant
    Filed: February 18, 2008
    Date of Patent: August 28, 2012
    Assignee: Magaldi Ricerche E Brevetti S.R.L.
    Inventor: Mario Magaldi
  • Publication number: 20110262323
    Abstract: The present invention relates to processes and apparatuses for hydromethanating a vanadium-containing carbonaceous feedstock while recovering at least a portion of the vanadium content originally present in the carbonaceous feedstock.
    Type: Application
    Filed: April 26, 2011
    Publication date: October 27, 2011
    Applicant: GREATPOINT ENERGY, INC.
    Inventors: Alkis S. Rappas, Robert A. Spitz
  • Publication number: 20110139628
    Abstract: The present invention concerns a method for producing calcium carbonate containing the steps of extraction of alkaline industrial waste or by-products using as a first extraction solvent an aqueous solution of a salt formed from a weak acid and a weak base, whereby a vanadium-enriched first residue is allowed to settle and a calcium-rich first filtrate is formed, filtration, whereby the first filtrate is separated from the first residue, carbonation of the calcium-rich first filtrate using a carbonation gas, whereby calcium carbonate precipitates and a second filtrate is formed, and a second filtration, whereby the calcium carbonate is separated from the second filtrate. Further, the present invention concerns a method for extracting calcium carbonate and vanadium from alkaline industrial waste or by-products.
    Type: Application
    Filed: May 29, 2009
    Publication date: June 16, 2011
    Applicant: Aalto University Foundation
    Inventors: Sebastian Teir, Sanni Eloneva, Hannu Revitzer, Ron Zevenhoven, Justin Salminen, Carl-Johan Fogelholm, Esko Poylio
  • Patent number: 7846404
    Abstract: A method is disclosed for separating and recovering base metals from a used hydroprocessing catalyst originating from Group VIB and Group VIII metals and containing at least a Group VB metal. In one embodiment, the used catalyst is contacted with an ammonia leaching solution to dissolve and separate the Group VIB and VIII metals from the Group VB metal complex and coke associated with the used catalyst. The resulting Group VIB and VIII metal containing solution is processed through at least two additional precipitation and liquid/solid separation steps to produce, in separate processing streams, a Group VIB metal product solution (such as ammonium molybdate) and a Group VIII metal product solution (such as nickel sulfate). Additionally, two separate filtrate streams are generated from liquid-solid separation steps, which filtrate streams are combined and subjected to hydrolysis and oxidation (oxydrolysis) to generate a purified ammonium sulfate solution for further processing, such as for fertilizer.
    Type: Grant
    Filed: December 19, 2008
    Date of Patent: December 7, 2010
    Assignee: Chevron U.S.A. Inc.
    Inventors: Rahul S. Bhaduri, John Stiksma, Roman Berezowsky
  • Patent number: 7837960
    Abstract: A method is disclosed for separating and recovering base metals from a used hydroprocessing catalyst originating from Group VIB and Group VIII metals and containing at least a Group VB metal.
    Type: Grant
    Filed: December 19, 2008
    Date of Patent: November 23, 2010
    Assignee: Chevron U.S.A. Inc.
    Inventors: Rahul S. Bhaduri, John Stiksma, Roman Berezowsky
  • Publication number: 20100226838
    Abstract: The present invention relates to a process for the removal of metal catalyst degradation products from a bleed stream of a catalytic chemical reaction process, wherein the catalyst is based on a metal selected from those in group VIII of the periodic table, chromium, copper, molybdenum, tungsten, rhenium, vanadium, titanium and zirconium, said process comprising treatment of the bleed stream with an alkali metal carbonate or ammonium carbonate source to form a solid complex or an aqueous solution of said solid complex, and removal of the solid complex or the aqueous solution of said solid complex from the bleed stream.
    Type: Application
    Filed: May 28, 2008
    Publication date: September 9, 2010
    Inventors: Anand Kumar Bachasingh, Arie Van Zon
  • Patent number: 7737068
    Abstract: A process for recovering catalytic metals from fine catalyst slurried in heavy oil comprises pyrolizing fine catalyst slurried in heavy oil to provide one or more lighter oil products and a coke-like material and recovering catalytic metals from the coke-like material.
    Type: Grant
    Filed: December 20, 2007
    Date of Patent: June 15, 2010
    Assignee: Chevron U.S.A. Inc.
    Inventors: Christopher A. Powers, Donald H. Mohr, Bruce E. Reynolds, Jose Guitian Lopez
  • Patent number: 7736607
    Abstract: The process of this invention is directed to the removal of metals from an unsupported spent catalyst. The catalyst is subjected to leaching reactions. Vanadium is removed as a precipitate, while a solution comprising molybdenum and nickel is subjected to further extraction steps for the removal of these metals. Molybdenum may alternately be removed through precipitation.
    Type: Grant
    Filed: December 30, 2008
    Date of Patent: June 15, 2010
    Assignee: Chevron U.S.A. Inc
    Inventor: Paul J. Marcantonio
  • Patent number: 7718147
    Abstract: The invention relates to a process for the chemical beneficiation of raw material containing tantalum-niobium such as wastes, scoria, concentrates and ores.
    Type: Grant
    Filed: January 24, 2006
    Date of Patent: May 18, 2010
    Assignee: Krupinite Corporation Ltd.
    Inventor: Alexander Krupin
  • Patent number: 7485267
    Abstract: The process of this invention is directed to the removal of metals from an unsupported spent catalyst. The catalyst is subjected to leaching reactions. Vanadium is removed as a precipitate, while a solution comprising molybdenum and nickel is subjected to further extraction steps for the removal of these metals. Molybdenum may alternately be removed through precipitation.
    Type: Grant
    Filed: July 29, 2005
    Date of Patent: February 3, 2009
    Assignee: Chevron U.S.A. Inc.
    Inventor: Paul J. Marcantonio
  • Patent number: 7241911
    Abstract: The present invention relates to novel, water-soluble niobium compounds, a process for their preparation and their formulations.
    Type: Grant
    Filed: September 29, 2005
    Date of Patent: July 10, 2007
    Assignee: H. C. Starck GmbH & Co. KG
    Inventors: Karsten Beck, Hady Seyeda, Udo Sulkowski, Axel Rosenkranz
  • Patent number: 7182925
    Abstract: A method for the dissolution and purification of tantalum ore and synthetic concentrates is described. The method preferably uses ammonium bifluoride as the fluoride source in place of the hydrofluoric acid used in the conventional methods. Other fluoride compounds such as NaF, KF, and CaF2 may be used alone or in combination with ammonium bifluoride. The tantalum concentrate and fluoride source are combined with sulfuric acid to form a solution containing tantalum values and impurities. The tantalum values are then separated from the impurities by solvent extraction.
    Type: Grant
    Filed: April 22, 2004
    Date of Patent: February 27, 2007
    Assignee: Osram Sylvania Inc.
    Inventors: Raj P. Singh Gaur, Robert G. Mendenhall
  • Patent number: 7182926
    Abstract: A process for economically separating and recovering valuable metal components, with few kinds of chemicals being used, with no waste water that causes environmental pollution being discharged, and also perfectly no by-products being formed by means of simple steps.
    Type: Grant
    Filed: April 22, 2004
    Date of Patent: February 27, 2007
    Assignee: Y. K. YSK Technosystem
    Inventor: Toshiaki Akahoshi
  • Patent number: 7083774
    Abstract: A process for producing a vanadyl sulphate solution (VOSO4) comprises forming a suspension of vanadium trioxide (V2O3) in a sulphuric acid solution and contacting the V2O3 suspension with a strong oxidising agent under controlled conditions to produce the VOSO4 solution. A preferred oxidising agent is hydrogen peroxide, which is added very slowly to the V2O3 suspension due to the violent nature of the reaction.
    Type: Grant
    Filed: May 26, 2003
    Date of Patent: August 1, 2006
    Assignee: Highveld Steel and Vanadium Corporation Limited
    Inventors: Andries Gerhardus Dormehl, Patrick Albert Monaghan
  • Patent number: 7052660
    Abstract: There is disclosed a wet-processing method for combustion ashes of petroleum fuels, comprising a slurry preparation step of preparing a slurry of the combustion ashes; a metal oxidation step of preparing a slurry containing ammonium metavanadate; a solid/liquid separation step of removing solids from the slurry containing ammonium metavanadate; a double decomposition step for ammonium sulfate, of adding a magnesium compound to an aqueous ammonium sulfate solution recovered from the solid/liquid separation step; and an ammonia recovery step of recovering ammonia from a reaction solution recovered from the double decomposition step. The above metal oxidation step is conducted while controlling an ammonium sulfate concentration of the aqueous solution to 20 to 45% by weight and the temperature of the aqueous solution to not more than 50° C., and the above solid/liquid separation step is conducted using a specific solid/liquid separator while controlling the temperature of the slurry to not more than 40° C.
    Type: Grant
    Filed: February 27, 2002
    Date of Patent: May 30, 2006
    Assignee: Kashima-Kita, Electric Power Corporation
    Inventor: Akira Sakuma
  • Publication number: 20040213717
    Abstract: The present invention provides a process for economically separating and recovering valuable metal components, with no many kinds of chemicals being used, with no waste water that causes environmental pollution being discharged, and also perfectly no by-products being formed by means of simple steps.
    Type: Application
    Filed: April 22, 2004
    Publication date: October 28, 2004
    Inventor: Toshiaki Akahoshi
  • Patent number: 6764663
    Abstract: A process for preparing a reconstituted vanadyl sulphate/vanadous sulphate solution for use as an electrolyte in a vanadium redox battery is disclosed. The process includes preparing a starting material including a vanadyl sulphate/vanadous sulphate solution, evaporating the starting material by applying heat to form vanadyl sulphate/vanadous sulphate crystals, and re-dissolving the vanadyl sulphate/vanadous sulphate crystals with a volume of de-ionized water to form a reconstituted vanadyl sulphate/vanadous sulphate solution having substantially the same chemical composition at the starting material. A process for preparing a vanadyl sulphate/vanadous sulphate starting material from a vanadium bearing ore material, particularly a titaniferous magnetite ore material is also disclosed.
    Type: Grant
    Filed: August 10, 2001
    Date of Patent: July 20, 2004
    Assignee: Highveld Steel and Vanadium Corporation Limited
    Inventors: Patrick Albert Monaghan, Ivan Strydom, Andries Gerhardus Dormehl
  • Publication number: 20030219367
    Abstract: A process for recovering the vanadium present in the chromium ore chromite. as ammonium metavanadate, as a by-product of the fusion of the chromium ore with alkali and its work-up to produce sodium chromate solution and sodium dichromate.
    Type: Application
    Filed: April 1, 2003
    Publication date: November 27, 2003
    Applicant: Bayer Aktiengesellschaft
    Inventors: Rainer Weber, Hans-Dieter Block, Michael Batz
  • Patent number: 6652819
    Abstract: A process for the production of a vanadium compound from carbonaceous residues containing vanadium, which includes the steps of: (a) combusting the carbonaceous residues at a temperature of 500-690° C. in an oxygen-containing gas to form vanadium-containing combustion residues; (b) heating the vanadium-containing combustion residues at a temperature T in ° C. under an oxygen partial pressure of at most T in kPa wherein T and P meet with the following conditions: log10(P)=−3.45×10−3×T+2.21 500≦T≦1300 to obtain a solid product containing less than 5% by weight of carbon and vanadium at least 80% of which is tetravalent vanadium oxide; (c) selectively leach tetravalent vanadium ion with sulfuring acid at pH in the range of 1.5-4; (d) separating a liquid phase from the leached mixture; (e) adding an alkaline substance to the liquid phase to adjust the pH thereof in the range of 4.5-7.
    Type: Grant
    Filed: June 5, 2001
    Date of Patent: November 25, 2003
    Assignee: Chiyoda Corporation
    Inventors: Yoshimi Shiroto, Ataru Wakabayashi
  • Publication number: 20030161770
    Abstract: There is disclosed a wet-processing method for combustion ashes of petroleum fuels, comprising a slurry preparation step of preparing a slurry of the combustion ashes; a metal oxidation step of preparing a slurry containing ammonium metavanadate; a solid/liquid separation step of removing solids from the slurry containing ammonium metavanadate; a double decomposition step for ammonium sulfate, of adding a magnesium compound to an aqueous ammonium sulfate solution recovered from the solid/liquid separation step; and an ammonia recovery step of recovering ammonia from a reaction solution recovered from the double decomposition step. The above metal oxidation step is conducted while controlling an ammonium sulfate concentration of the aqueous solution to 20 to 45% by weight and the temperature of the aqueous solution to not more than 50° C.
    Type: Application
    Filed: September 18, 2002
    Publication date: August 28, 2003
    Inventor: Akira Sakuma
  • Patent number: 6592830
    Abstract: The invention relates to a process for treating tantalum and/or niobium containing raw materials such as wastes, slags, concentrates and ores. The tantalum and/or niobium containing raw materials are processed by repeated use of a solution of ammonium fluoride. From the tantalum and niobium containing aqueous solution a mixture of fluorides and oxide fluorides of tantalum and niobium are transformed into a firm condition. At an extraction stage pure, aqueous solutions containing fluoro acid complexes of niobium and fluoroammonium complexes of tantalum are obtained. From these tantalum and niobium are obtained as oxides in pure form by precipitating them as fluoride containing oxide hydrates by addition of ammonia. The obtained oxide hydrates are transformed into pure oxides by calcining at high temperatures.
    Type: Grant
    Filed: April 17, 2001
    Date of Patent: July 15, 2003
    Inventors: Aleksandr Krupin, Nikolai Galaganov
  • Patent number: 6333012
    Abstract: A process is provided for preparing ammonium metavanadate from the combustion ashes resulting from the combustion of petroleum fuels in a boiler by using the ammonium sulfate and vanadium components in the combustion ash. Water is added to the combustion ash to form a slurry. The solids are removed from the slurry. Ammonia and an oxidizing gas, such as air, oxygen or ozone, are added to the aqueous solution obtained from the slurry to oxidize the vanadium, thereby producing an aqueous solution containing ammonium metavanadate. The ammonium metavanadate is crystallized and recovered from the aqueous solution. Calcium hydroxide or calcium oxide is injected into the aqueous solution and reacts with the ammonium sulfate to produce gypsum and ammonia. This gypsum and ammonia containing solution is flowed down a packed column, where it is counter-currently contacted with air or steam which strips the ammonia out of the solution.
    Type: Grant
    Filed: January 14, 2000
    Date of Patent: December 25, 2001
    Assignee: Kashima-Kita Electric Power Corp.
    Inventors: Toshiaki Akahoshi, Akira Sakuma, Aritoshi Inoue, Masami Iijima
  • Patent number: 6180072
    Abstract: There is provided a process to reclaim metals from catalysts, said process comprising collecting one or more catalyst containing at least one metal sulfide; leaching the catalyst in an atmospheric leach step; separating the leached slurry into a first liquid stream and a first solid; leaching the first solid in a pressure leach process; separating the second leached slurry into a second liquid stream and a second solid; collecting the first and second liquid streams; oxidizing the combined liquid stream; cooling the oxidized liquid stream; adjusting the pH of the oxidized liquid stream; contacting the cooled oxidized liquid stream with an organic solvent containing an extractant; stripping the soluble metal species from the organic phase; adjusting the pH of the aqueous phase to selectively precipitate at least one metal as a metal salt; and separating the metal salt from the aqueous phase.
    Type: Grant
    Filed: May 6, 1999
    Date of Patent: January 30, 2001
    Assignee: Shell Oil Company
    Inventors: Jack Thomas Veal, Kevin Arnold Andersen, Ruth Mary Kowaleski
  • Patent number: 5635146
    Abstract: A method is disclosed for the dissolution and purification of tantalum pentoxide. The impure tantalum pentoxide is reacted with a potassium-containing compound to form potassium tantalate. The potassium tantalate is optionally slurried with sulfuric acid and dissolved in an HF medium. The solution is suitable for purification by conventional ion exchange or solvent extraction methods. A potassium fluorotantalate precipitate may also be formed by adding KCl to the solution. The fluorotantalate precipitate may be further processed into a pure tantalum pentoxide by suspending the precipitate in an aqueous solution optionally containing a chelating agent and adding ammonium hydroxide to form ammonium tantalum oxide which can then be converted to tantalum pentoxide by calcining at high temperature.
    Type: Grant
    Filed: November 30, 1995
    Date of Patent: June 3, 1997
    Assignee: Osram Sylvania Inc.
    Inventors: Raj P. Singh, Michael J. Miller
  • Patent number: 5368762
    Abstract: Tri- and tetravalent vanadium solutions suitable for a redox battery are produced as follows. Vanadium pentaoxide or ammonium vanadium is reduced in the presence of a concentrated sulfuric acid and a reducer, thus producing a solution containing tetravalent vanadium. At least a portion of the trivalent vanadium solution is heated to 180.degree.-250.degree. C., thus producing a trivalent vanadium compound. If the trivalent compound produced is a solid, it is collected and solubilized in water and/or sulfuric acid. Then, unreacted sulfur is filtered out, thus obtaining a trivalent vanadium solution.
    Type: Grant
    Filed: April 1, 1993
    Date of Patent: November 29, 1994
    Assignee: Kashima-Kita Electric Power Corporation
    Inventors: Kanji Sato, Masato Nakajima, Ko Magome
  • Patent number: 5209910
    Abstract: Improved solvent extraction recovery of tantalum and niobium oxides from an acid solution of raw materials containing such oxides wherein the charged organic solvent [e.g., MIBK] is washed out (a) with 8-16N sulfuric acid and then (b) with water or dilute HF. This avoids the use of a second mineral acid addition after digestion by HF of raw materials (and avoids problems attendant to use a second mineral acid).
    Type: Grant
    Filed: June 24, 1991
    Date of Patent: May 11, 1993
    Assignee: Hermann C. Starck GmbH & Co. KG
    Inventors: Walter Bludssus, Joachim Eckert
  • Patent number: 5194232
    Abstract: Fluorine content of tantalum and niobium hydroxides is reduced to under 0.5 weight % by washing such hydroxide precipitates (as obtained by HF digestion and solvent extraction) with dilute ammonia (1 to 10%) and then water in two washing stages. The first washing stage includes a partial neutralization and the used wash water of the second stage is advantageously recycled, after adjustment of its ammonia concentration, for use as the first stage washing liquid.
    Type: Grant
    Filed: August 27, 1991
    Date of Patent: March 16, 1993
    Assignee: Hermann C. Starck Berlin GmbH & Co. KG
    Inventors: Walter Bludssus, Erk-Rudiger Feuerhahn, Horst Zimmermann
  • Patent number: 4978511
    Abstract: Vanadium is selectively recovered from vanadium-containing phosphoric acid solutions also containing metals other than vanadium by selectively converting the dissolved vanadium to a vanadate compound insoluble in the phosphoric acid solution and separating the resulting insoluble vanadate compound, free of other metal compounds, from the phosphoric acid solution. The dissolved vanadium can be converted to an insoluble vanadate by reaction with oxidants and/or cations which form phosphoric acid-insoluble vanadates. These methods can be employed to selectively recover vanadium from phosphoric acid solutions containing other metals. They also can be employed to recover vanadium compounds from ores, scrap metal, and other vanadium sources by dissolving the vanadium from the vanadium source in phosphoric acid and recovering the vanadium as an insoluble compound from the phosphoric acid as described.
    Type: Grant
    Filed: July 20, 1989
    Date of Patent: December 18, 1990
    Assignee: Union Oil Company of California
    Inventor: Donald C. Young
  • Patent number: 4948570
    Abstract: The process for removing tantalum values from niobium values wherein a NbCl.sub.5 /TaCl.sub.5 charge mixture having a molar ratio from about 10/1 to about 10,000/1 is mixed with a 8N to 20N aqueous HCl solution at a total charge concentration of from about 50 to about 150 parts/100 parts by weight of the HCl solution to form a hydrolysis system, and wherein at least the surface of the hydrolysis system is contacted with air or a gas-containing air for a period of time within which a precipitate settles out at an average rate of from about 0.1 to about 6.0% by weight of the initial solids charge per hour.
    Type: Grant
    Filed: July 11, 1989
    Date of Patent: August 14, 1990
    Assignee: Teledyne Industries, Inc.
    Inventor: James A. Sommers
  • Patent number: 4942024
    Abstract: Refining of either niobium hydroxide or tantalum hydroxide containing transition metals as impurities is accomplished easily and economically by dissolving the metal hydroxide in an aqueous solution of either hydrofluoric acid or oxalic acid, adjusting the pH of the solution to 1 to 4 and adding ammonium pyrrolidinedithiocarbamate (APDC) to the solution while maintaining the temperature of the solution below 60.degree. C. The addition of APDC causes the transition metals to simultaneously precipitate as coordination compounds. The minimum amount of APDC is 0.05 wt % of Nb.sub.2 O.sub.5 or Ta.sub.2 O.sub.5 that can be formed from Nb or Ta contained in the solution. After the treatment with APDC the pH of the solution is raised to 6 or above to precipitate the refined metal hydroxide.
    Type: Grant
    Filed: June 2, 1989
    Date of Patent: July 17, 1990
    Assignee: Central Glass Company, Limited
    Inventors: Hiromi Sasaki, Tadasi Tanaka, Yasusi Muneno
  • Patent number: 4913885
    Abstract: Vanadium values useful for catalyst regeneration are recovered from compositions/materials comprised thereof, typically spent V.sub.2 O.sub.5 catalysts, by intimately contacting an aqueous suspension of such a material with a gaseous admixture of sulfur dioxide and oxygen, whereby a phase separation thus results, and recovering an aqueous phase constituting a solution of vanadium values.
    Type: Grant
    Filed: April 27, 1988
    Date of Patent: April 3, 1990
    Assignee: Rhone-Poulenc Chimie
    Inventors: Francoise Seon, Michel Ries
  • 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: 4883601
    Abstract: A process for purifying an aqueous, hydrogen sulfide-scrubbing solution which contains a water-soluble transition metal component, such as a vanadium component or an iron component, in addition to at least one water-soluble organic compound, such as an aromatic sulfonate or an alkanolamine, in which the scrubbing solution is mixed with particles of a spent solid catalyst containing molybdenum and aluminum and a basic aqueous solution, preferably a solution comprising sodium aluminate, to form a slurry which is subsequently contacted with an oxygen-containing gas under conditions such that the molybdenum in the catalyst is solubilized. Thereafter, molybdenum is precipitated from the solution along with the water-soluble transition metal component and a wastewater substantially free of the transition metal component and the organic compound originally present in the scrubbing solution is recovered.
    Type: Grant
    Filed: August 30, 1988
    Date of Patent: November 28, 1989
    Assignee: Union Oil Company of California
    Inventors: Jeffery W. Koepke, Dennis D. Delaney
  • Patent number: 4851199
    Abstract: Vanadium is recovered from vanadium-containing phosphoric acid solutions by adjusting the pH so as to convert the dissolved vanadium to a simple vanadate compound which is insoluble in the phosphoric acid solution at the adjusted pH and separating the resulting insoluble simple vanadate compound from the phosphoric acid solution. The vanadium dissolved in the phosphoric acid solution can be converted to insoluble simple vanadates by reaction with oxidants and/or cations which form phosphoric acid-insoluble simple vanadates. These methods can be employed to selectively recover vanadium from phosphoric acid solutions containing other metals. They also can be employed to recover vanadium compounds from ores, scrap metal, and other vanadium sources by dissolving the vanadium from the vanadium source in phosphoric acid and recovering the vanadium as an insoluble simple vanadate from the phosphoric acid as described.
    Type: Grant
    Filed: October 19, 1987
    Date of Patent: July 25, 1989
    Assignee: Union Oil Company of California
    Inventor: Donald C. Young
  • Patent number: 4816236
    Abstract: A process is provided for the recovery of vanadium and nickel values from petroleum residues and, in particular, from Flexicoke. In the process, Flexicoke is blended with an alkali metal source, such as sodium sulfate or sodium carbonate, and then roasted in an oxygen-containing gas until carbon is removed and a fused mixture is obtained. Thereafter, the vanadium is leached from the mixture with an aqueous solution, and nickel is contained in solids remaining from the leaching.
    Type: Grant
    Filed: December 18, 1987
    Date of Patent: March 28, 1989
    Assignee: U.S. Vanadium Corporation
    Inventor: Harry E. Gardner
  • Patent number: 4814150
    Abstract: A process for the high-yield recovery of vanadium from petroleum combustion residues, wherein these residues are: (a) subjected to attach with sodium hydroxide in the presence of an oxidizer, or (b) impregnated with sodium hydroxide, dried at 100.degree.-250.degree. C. and leached with water, to selectively extract vanadium with high yields. The vanadium is precipitated from the alkaline extract by adding H.sub.2 SO.sub.4 up to pH.apprxeq.2 and an ammonium salt. The precipitated ammonium polyvanadate is calcinated to vanadium pentoxide.
    Type: Grant
    Filed: July 13, 1987
    Date of Patent: March 21, 1989
    Assignee: Ente Minerario Siciliano
    Inventors: Francesco Corigliano, Sebastiana Di Pasquale, Patrizia Primerano, Cesare Zipelli
  • Patent number: 4640823
    Abstract: A process is provided for the recovery of vanadium values from vanadium-bearing residues, such as fly ash, boiler ash and scrubber residues from the combustion of crude oil fractions. The process employs a combination of alkaline metal bases, such as sodium carbonate and sodium hydroxide.
    Type: Grant
    Filed: March 13, 1986
    Date of Patent: February 3, 1987
    Assignee: U.S. Vanadium Corporation
    Inventor: John B. Goddard
  • Patent number: 4637920
    Abstract: The object of this invention is a process for separating metal compounds, even in small percentages, from dusts and sludges, by reduction.The process may be successfully applied to the selective separation of vanadium pentoxide contained in small fractions in the ashes of heavy fuels, as well as to the separation and/or passivation of chromium compounds, of which the polluting characteristics are well-known.Separation is obtained by means of a reduction tower containing preferably iron scraps or shavings, adjusting on one side the pH of the input solutions according to their compositions, and on the other side the speed with which the solution passes through the reduction tower, so as to obtain a specific pH value of the output, again depending on the type of metal to be treated (FIG. 2).
    Type: Grant
    Filed: May 14, 1985
    Date of Patent: January 20, 1987
    Assignee: VA.NI.M S.r.l
    Inventor: Adolfo Piuma
  • Patent number: 4587109
    Abstract: The invention relates to a process for recovering and purifying the molybdenum from a solution containing more molybdenum than vanadium.The process of the invention comprises the step of contacting the solution which contains molybdenum and vanadium, originally at a pH at least equal to 11 with an excess of an ammonium salt sufficient to precipitate the greatest part of vanadium in the form of solid ammonium vanadate, this excess being yet hot higher than a value such that after precipitation of vanadium, the quantity of ammonium having not reacted with the vanadate would be over a concentration which would account for risks of precipitating also molybdenum which is contained in the liquid phase of the supernatant.The molybdenum which is obtained is of industrial grade.
    Type: Grant
    Filed: July 8, 1983
    Date of Patent: May 6, 1986
    Assignee: Compagnie Generale des Matieres Nucleaires (COGEMA)
    Inventors: Georges Lyaudet, Jean Vial
  • Patent number: 4554138
    Abstract: A process for enhancing recovery of metals, especially cobalt, from spent hydroprocessing catalysts when the spent catalyst particles are first roasted at between 400.degree. C. and 600.degree. C. and then contacted with a first aqueous solution of ammonia and an ammonium salt to recover nickel, cobalt, molybdenum, tungsten, and vanadium. The once-leached spent hydroprocessing catalysts are again leached by contacting them with a second aqueous solution of ammonium sulfate at a pH of 1 to 4.
    Type: Grant
    Filed: October 30, 1984
    Date of Patent: November 19, 1985
    Assignee: Chevron Research Company
    Inventor: Paul J. Marcantonio
  • Patent number: 4551315
    Abstract: A method of recovering vanadium from an aqueous ammonium bicarbonate solvent strip solution is disclosed. The method includes adding sulfuric acid to the aqueous ammonium bicarbonate solution followed by addition of ammonia or ammonium hydroxide to precipitate out the vanadium.
    Type: Grant
    Filed: November 26, 1984
    Date of Patent: November 5, 1985
    Assignee: Chevron Research Company
    Inventor: Paul J. Marcantonio
  • Patent number: 4544533
    Abstract: A method of recovering vanadium from an aqueous ammonium bicarbonate solvent strip solution is disclosed. The method includes heating the aqueous ammonium bicarbonate solution at a temperature of from 70.degree. C. to 100.degree. C., followed by addition of sulfuric acid to control the pH in the range of from 6.5 to 8.5 and addition of ammonium sulfate to precipitate out the vanadium.
    Type: Grant
    Filed: November 26, 1984
    Date of Patent: October 1, 1985
    Assignee: Chevron Research Company
    Inventor: Paul J. Marcantonio
  • Patent number: 4477416
    Abstract: A process is provided for extracting vanadium values from a vanadium-bearing ore in which a carbonaceous material is added to a salt roast mixture containing ore and an alkali metal salt, e.g., NaCl. The mixture is subjected to roast temperatures (e.g., 825.degree. C.) for a period of time sufficient to burn off substantially all of the carbon in the mixture. The carbonaceous material is preferably a vanadium-containing carbon source, e.g., residue from the combustion of heavy petroleum oil.
    Type: Grant
    Filed: September 27, 1982
    Date of Patent: October 16, 1984
    Assignee: Union Carbide Corporation
    Inventor: John B. Goddard
  • Patent number: 4420464
    Abstract: A carbonaceous material containing vanadium is reacted with an oxidizing gas in a molten salt pool containing an alkali metal carbonate. Vanadium values present in the carbonaceous material are converted to water-soluble vanadium compounds which are recovered from the melt and reacted with a strong acid to precipitate the vanadium values as insoluble vanadates. The vanadates are recovered as product or optionally further converted to vanadium pentoxide.
    Type: Grant
    Filed: October 26, 1981
    Date of Patent: December 13, 1983
    Assignee: Rockwell International Corporation
    Inventor: Kenneth M. Barclay
  • Patent number: 4389378
    Abstract: Vanadium values are recovered from cokes and ashes derived from heavy oils by a novel process comprising heating in the presence of alkali metal sulphate, contacting the resulting solid residue with water and recovering the vanadium values dissolved therein.
    Type: Grant
    Filed: December 24, 1981
    Date of Patent: June 21, 1983
    Assignee: Gulf Canada Limited
    Inventor: Lois L. McCorriston
  • Patent number: 4344924
    Abstract: Chromium and vanadium can be co-extracted from alkaline solutions or leach liquors containing these metals using quaternary amine solvent mixtures. The alkaline leach liquors usually are derived by leaching of calcined ores or concentrates. The loaded solvent mixture is scrubbed with chromium solution to remove all metals except chromium, and the chromium is then recovered from the solvent phase. The vanadium can be recovered from the scrub liquor. Recovery of aluminum is also possible.
    Type: Grant
    Filed: August 11, 1980
    Date of Patent: August 17, 1982
    Assignee: Canadian Patents & Development Ltd.
    Inventors: Bernard H. Lucas, Gordon M. Ritcey
  • Patent number: 4216053
    Abstract: Solid particles of ammonium decavanadate are recovered from an aqueous ammonium decavanadate solution by atomizing the solution and heating the fine droplets to vaporize the water constituent and form solid particles of ammonium decavanadate which are quickly cooled.
    Type: Grant
    Filed: October 6, 1978
    Date of Patent: August 5, 1980
    Assignee: Union Carbide Corporation
    Inventors: John L. Powell, Peter C. Rekemeyer, Earl E. Falk