Removing Undesirable Matter From Vapor Patents (Class 423/77)
  • Patent number: 8309042
    Abstract: The disclosure provides a process for recycling ore in the chloride process, without the build-up of silica-containing gangue in the chlorination reactor.
    Type: Grant
    Filed: January 23, 2008
    Date of Patent: November 13, 2012
    Assignee: E I du Pont de Nemours and Company
    Inventors: Matthew Donnel Eisenmann, Jorge Lavastida, Timothy Josiah McKeon, James Elliott Merkle, Jr.
  • Patent number: 7780931
    Abstract: Process for preparing TiO2 powders starting from a liquid comprising chlorinated titanium compounds, the process comprising: a) atomizing said liquid and reacting the atomized liquid with a flow of steam and air at a temperature of 100-250° C. for converting said chlorinated titanium compounds to titanium dioxide TiO2; b) the gaseous phase and the entrained TiO2 powders obtained from step a) are then fed to an oven operated at a temperature in the range 400-900° C. to remove the residual organic compounds and hydrochloridic acid from said powders.
    Type: Grant
    Filed: November 3, 2005
    Date of Patent: August 24, 2010
    Assignee: Basell Poliolefine Italia s.r.l.
    Inventors: Anna Fait, Arrigo Arletti, Lucia Caiazzo
  • Patent number: 7368096
    Abstract: The disclosure is directed to a process for isolating solids from a purification purge stream comprising an impurity present as a solid, wherein the purification purge stream is substantially free of chlorides other than titanium tetrachloride and vanadium chloride, the process comprising the steps of: (a) atomizing the purification purge stream comprising titanium tetrachloride as a liquid and an impurity present as a solid; (b) drying solids in the atomized purification purge stream by contacting the atomized stream with a titanium tetrachloride vapor stream such that the combined streams reach a temperature of at least about 140° C. to vaporize the liquid titanium tetrachloride, wherein the titanium tetrachloride vapor is substantially free of chlorides other than those of titanium and vanadium, and substantially free of non-condensable gases comprising CO, CO2, N2, or mixtures thereof; and (c) separating the impurity present as a solid from the vaporized titanium tetrachloride.
    Type: Grant
    Filed: June 7, 2005
    Date of Patent: May 6, 2008
    Assignee: E.I. du Pont de Nemours and Company
    Inventors: Xuqing Gu, Stephen Erwin Lyke, Steve Mirabella, Joseph M. Shekiro, Jr., Jodi Lynn Witt
  • Patent number: 7153488
    Abstract: The present invention is directed to the suppression of the formation noxious compounds such as furans. According to the present invention, a venturi device is used to rapidly quench a chlorinator reaction gas. The rapid quench minimizes the resonance time that furan precursors are at conditions conducive to furan formation.
    Type: Grant
    Filed: August 3, 2004
    Date of Patent: December 26, 2006
    Assignee: Millennium Inorganic Chemicals, Inc.
    Inventors: Thomas Messer, Peter Carter
  • Patent number: 6770254
    Abstract: This invention relates to an improved process for removing trace levels of Group IVb contaminants from a Group IVb metal tetrahalide of and particularly to a process for removing zirconium tetrachloride from titanium tetrachloride. The improvement resides in contacting a titanium tetrachloride feedstock containing trace impurities of zirconium tetrachloride or hafnium tetrachloride with a sufficient amount of titanium hydride to convert any zirconium tetrachloride or hafnium tetrachloride to a lower volatile compound. The resultant mixture is distilled and the titanium tetrachloride separated from the lower volatile zirconium or hafnium compounds.
    Type: Grant
    Filed: January 17, 2002
    Date of Patent: August 3, 2004
    Assignee: Air Products and Chemicals, Inc.
    Inventors: Heather Regina Bowen, David Allen Roberts
  • Patent number: 6399033
    Abstract: An improvement to the chloride process of making titanium dioxide. By recycling some of the cyclone dust, the yield in the chlorination of titanium-containing raw materials can be increased. In order to prevent silica accumulation in the fluidized bed, the cyclone dust is divided into two fractions. An economic solution is described of a single-stage separation of the cyclone dust in a hydrocyclone, the majority of the titanium dioxide occurring in the hydrocyclone underflow, although the separation is not sharp. By grinding and drying the solids from the hydrocyclone underflow, the titanium dioxide particles returned to the lower region of the fluidized-bed reactor are rapidly chlorinated, while the quartz and coke particles are rapidly discharged again from the fluid bed, so that no silica contamination occurs.
    Type: Grant
    Filed: November 3, 1995
    Date of Patent: June 4, 2002
    Assignee: Kronos, Inc.
    Inventor: Achim Hartmann
  • Patent number: 6136060
    Abstract: A method for refining a titanium metal containing ore such as rutile or illmenite or mixtures to produce titanium ingots or titanium alloys and compounds of titanium involves production of titanium tetrachloride as a molten slag, by processing the ore in a chlorination procedure and removing various impurities by a distillation or other procedure to form a relatively pure titanium tetrachloride (TiCl.sub.4). Thereafter, the titanium tetrachloride is introduced into the plasma focal point of a plasma reactor in a molten sodium environment for the initial reduction of gas phase titanium into titanium molten drops which are collected by a set of skulls. Thereafter, further processing are carried out in higher vacuum and the titanium is heated by electron beam guns in order to maximize titanium purity and, in a final optional stage, alloying compounds are added under yet higher vacuum and high temperature conditions.
    Type: Grant
    Filed: October 16, 1998
    Date of Patent: October 24, 2000
    Inventor: Adrian A. Joseph
  • Patent number: 5437854
    Abstract: Zirconium tetrachloride containing hafnium tetrachloride is selectively reduced with liquid metallic tin to produce zirconium trichloride. The hafnium tetrachloride is then separated as a vapor from a slurry of zirconium trichloride and other solids, including stannous dichloride, in liquid metallic tin.
    Type: Grant
    Filed: June 27, 1994
    Date of Patent: August 1, 1995
    Assignee: Westinghouse Electric Corporation
    Inventors: Roy G. Walker, Carlos L. Aguilar
  • Patent number: 5411724
    Abstract: Aluminum can be removed from tetrahedral framework sites of zeolite frameworks and substituted with elements such as silicon, gallium, titanium or zirconium. The process involves three steps:(a) forming a mixture of the ammonium or alkaline metal form of the zeolite in the hydrated state and a crystalline ammonium fluoro-halo-metallate salt;(b) heating the mixture at elevated temperatures to remove the aluminum from the zeolite and to introduce the metal from the salt into the structure of the zeolitic component by solid-state reaction while forming a fluoro-halo-aluminate complex salt; and(c) removing the formed fluoro-halo-aluminate complex salt.
    Type: Grant
    Filed: June 2, 1993
    Date of Patent: May 2, 1995
    Assignee: W. R. Grace & Co.-Conn.
    Inventors: Herman K. Beyer, Gabriella Pal-Borbely
  • Patent number: 5372639
    Abstract: Disclosed is a process of using a bimodal distribution of scrubs in an externally cooled conduit during heat removal whereby a hot gaseous suspension containing pigmentary metal oxides is subjected to cooling. Effective heat transfer is provided. Pigmentary properties such as CBU and gloss are improved.
    Type: Grant
    Filed: September 3, 1993
    Date of Patent: December 13, 1994
    Assignee: E. I. du Pont de Nemours and Company
    Inventors: Raul A. Gonzalez, Charles D. Musick
  • Patent number: 5298227
    Abstract: A process and apparatus for the separation of vaporous heavy metal compounds from a carrier gas wherein the heavy metal compounds are cooled and desublimed. An apparatus for carrying out this process has a melting furnace with a discharge opening for a gas/ vapor mixture, which leads to a cooling device.Vaporous heavy metal compounds can be separated from a carrier gas on a large industrial scale. In addition, the apparatus for carrying out this process is easy to operate. The gas/vapor mixture is turbulently mixed immediately after the discharge from the furnace in a mixing section with cold air and is thus cooled. During this cooling, the vaporous heavy metal compounds desublime and are filtered as particles in a filter.
    Type: Grant
    Filed: August 18, 1989
    Date of Patent: March 29, 1994
    Assignee: Asea Brown Boveri Ltd.
    Inventors: Michael Hirth, Joachim Jochum, Harald Jodeit, Christian Wieckert
  • Patent number: 5266108
    Abstract: In the process for cooling the reaction products of the vapor phase oxidation of titanium tetrachloride to titanium dioxide comprising: (a) passing said reaction products through an externally cooled conduit, and (b) admixing with the reaction products particulate scrubbing material which removes solid deposits adhered to the interior walls of the conduit, the improvement characterized by:using as the scrubbing material about 0.5-15 percent by weight, based on the weight of titanium dioxide, of compacted particles of titanium dioxide pigment, said compacted particles of titanium dioxide pigment being produced by subjecting titanium dioxide pigment to sufficient pressure to form same.
    Type: Grant
    Filed: April 22, 1992
    Date of Patent: November 30, 1993
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Howard M. Hauck
  • Patent number: 5102637
    Abstract: A vapor stream from a sand chlorinator containing principally zirconium tetrachloride, hafnium tetrachloride and silicon tetrachloride contaminated with ferric chloride is purified by cooling the vapor to a temperature of about 335.degree. C. to about 600.degree. C. The cooled vapors flow through a gaseous diffusion separative barrier where a silicon tetrachloride vapor stream contaminated with metal chlorides flows from the separative barrier as a "fast" stream; ferric chloride is adsorbed by the separative barrier; and a vapor stream principally containing zirconium tetrachloride, hafnium tetrachloride and silicon tetrachloride is screened by the separative barrier.
    Type: Grant
    Filed: October 12, 1990
    Date of Patent: April 7, 1992
    Assignee: Westinghouse Electric Corp.
    Inventors: Thomas S. Snyder, Richard A. Stoltz
  • Patent number: 4933154
    Abstract: A ZrO.sub.2 powder of very fine particle size adapted especially for the making of high density ceramics is produced by chlorinating a zirconium source material, such as zircon sand, to produce crude ZrCl.sub.4 solids; the solids are dissolved to form a ZrOCl.sub.2 solution from which ZrOCl.sub.2 crystals are precipitated; the crystals are dried and milled to a desired particle size; and the crystal particles are subjected to direct oxidation under controlled conditions to produce a very fine ZrO.sub.2 powder especially adapted to the making of high density ceramics.
    Type: Grant
    Filed: January 30, 1987
    Date of Patent: June 12, 1990
    Assignee: Westinghouse Electric Corp.
    Inventor: Young J. Kwon
  • Patent number: 4913778
    Abstract: Removal of aluminum and iron impurities is accomplished using an absorbing column containing potassium or sodium chloride, producing an aluminum and iron chloride-rich bottoms product and purified Zr(Hf)Cl.sub.4 vapor at the top of the column. This invention is a continuous process for removing impurities of iron or aluminum chloride or both from vaporous zirconium chloride (or hafnium chloride or a mixture thereof). When iron is being removed from zirconium tetrachloride using potassium chloride, the process comprises: introducing impure zirconium chloride vapor into a middle portion of an absorbing column containing a potassium chloride-containing molten salt phase, the molten salt phase absorbing the iron chloride impurity to produce a zirconium chloride vapor stripped of iron chloride in the top portion of the column; introducing potassium chloride into a top portion of the column; controlling the top portion of the column to between 300.degree.-375.degree. C.
    Type: Grant
    Filed: January 2, 1989
    Date of Patent: April 3, 1990
    Assignee: Westinghouse Electric Corp.
    Inventors: Ernest D. Lee, David F. McLaughlin
  • Patent number: 4762696
    Abstract: A method of purificating titanium tetrachloride, comprising: heating a loose mass of catalytic metal to a temperature over 300.degree. C. approximately, introducing vapor of a crude titanium tetrachloride to contact with said metal, said chloride comprising a minor amount of metal oxychloride, causing a reaction to convert a substantial part of the oxychloride to substances which are less volatile than titanium tetrachloride, removing such substances in condensed state from the titanium tetrachloride in fluid state, and recovering thus purified titanium tetrachloride.
    Type: Grant
    Filed: May 7, 1987
    Date of Patent: August 9, 1988
    Inventor: Hiroshi Ishizuka
  • Patent number: 4731230
    Abstract: An improved process for the preparation of TiCl.sub.4 comprising(a) chlorinating a raw material containing titanium and vanadium impurities to produce a crude TiCl.sub.4 reaction product,(b) separating the crude reaction product into solid by-products and TiCl.sub.4 -containing liquid,(c) reacting the TiCl.sub.4 -containing liquid with a reducing agent whereby vanadium impurities are converted into solid compounds, and(d) separating TiCl.sub.4 from the solid vanadium compounds, is improved by adding solid products of the vanadium reduction reactions to the crude TiCl.sub.4 reaction product prior to the separating step (b).
    Type: Grant
    Filed: June 29, 1987
    Date of Patent: March 15, 1988
    Assignee: Bayer Aktiengesellschaft
    Inventors: Gunter Lailach, Walter Deissmann, Karl-Heinz Schultz
  • Patent number: 4578252
    Abstract: A method for preparing ultra-pure metal tetrafluorides in which 3d such as Fe impurities are separated from impure material by a combined vaporization-electrolytic separation procedure. Sublimation and distillation methods are disclosed in combination with electrolytic separation by both emf-series displacement (ESD) and direct melt electrolysis (DME).
    Type: Grant
    Filed: May 14, 1985
    Date of Patent: March 25, 1986
    Assignee: Hughes Aircraft Company
    Inventors: Ricardo C. Pastor, Morton Robinson
  • Patent number: 4540551
    Abstract: There is provided a multi stage process for nonselectively chlorinating a titaniferous ore containing iron to produce TiCl.sub.4. In this process a portion of the ore charge is subjected to conventional fluid bed chlorination to produce TiCl.sub.4 and FeCl.sub.2. A second portion is subdivided and submitted to chlorination in a dilute phase chlorination step using FeCl.sub.3 as the chlorinating agent to produce additional TiCl.sub.4. The FeCl.sub.3 is obtained by partial oxidation of the FeCl.sub.2 obtained in the first stage and/or second stage to yield Fe.sub.2 O.sub.3 and FeCl.sub.3. The product streams of TiCl.sub.4 are then combined for further treatment.
    Type: Grant
    Filed: March 1, 1985
    Date of Patent: September 10, 1985
    Assignee: SCM Corporation
    Inventors: James P. Bonsack, Semyon D. Fridman
  • Patent number: 4487677
    Abstract: An apparatus including a single electrolytic/reaction cell, for extraction of titanium sponge from rutile ore. Magnesium chloride is electrolytically separated into magnesium metal and chlorine gas within the cell. The chlorine gas produced is reacted with rutile ore and coke to produce titanium tetrachloride in a separate chlorinator and the product is directed to the cell subsequent to completion of electrolysis. Titanium tetrachloride is reacted with magnesium metal in the same cell where the magnesium is produced to form titanium sponge and magnesium chloride. The titanium sponge is separated within said cell with the magnesium chloride being recovered and recycled. Major impurities are separated by distillation. Plural electrolytic cells can be coupled to a single chlorinator in a continuous process. Very pure titanium sponge is produced with this self-replenishing process.
    Type: Grant
    Filed: April 11, 1983
    Date of Patent: December 11, 1984
    Assignee: Metals Production Research, Inc.
    Inventor: Andrew H. Murphy
  • Patent number: 4460550
    Abstract: Titanium tetrachloride is produced from titanium ore and reductant suspended in molten salt by the passage of chlorine therethrough. The titanium tetrachloride is scrubbed by passage through at least one scrubber of molten salt and oxidized to produce titanium oxide and chlorine. Chlorine is recaptured as a solute in cold titanium tetrachloride and then liberated and recycled.
    Type: Grant
    Filed: May 3, 1983
    Date of Patent: July 17, 1984
    Assignee: Kerr-McGee Chemical Corporation
    Inventor: Theodore A. Rado
  • Patent number: 4442075
    Abstract: A process of chlorinating titanium ore suspended with carbonaceous reductant in molten salt by passage of chlorine therethrough. Titanium tetrachloride produced is purified of by-product metal chlorides by their absorption in the salt as non-volatile double salts.
    Type: Grant
    Filed: March 30, 1983
    Date of Patent: April 10, 1984
    Assignee: Kerr-McGee Chemical Corporation
    Inventor: Theodore A. Rado
  • Patent number: 4440730
    Abstract: There is provided an improved process for the chlorination of particulate titaniferous ores using a particulate reactive carbon in a fluidized bed. The particulate reactive carbon is lignite char.
    Type: Grant
    Filed: November 17, 1982
    Date of Patent: April 3, 1984
    Assignee: SCM Corporation
    Inventor: James P. Bonsack
  • Patent number: 4435365
    Abstract: A process for producing titanium tetrachloride in which iron-titanium ore is leached in hydrochloric acid to produce a solid phase comprising upgraded titanium-containing material, and a spent liquid phase. Dissolved metal chlorides in the spent liquid phase are regenerated to produce hydrochloric acid in an acid regeneration zone. The titanium-containing material is chlorinated to produce a product stream containing titanium tetrachloride and entrained solids, including metal chloride. The entrained solids are recovered from the product stream and the metal chloride portion thereof is recycled to the acid regeneration zone.
    Type: Grant
    Filed: May 12, 1982
    Date of Patent: March 6, 1984
    Assignee: Kerr-McGee Chemical Corporation
    Inventor: Alan J. Morris
  • Patent number: 4329322
    Abstract: Vanadium impurities in chlorinated titaniferous materials are rendered easily removable by reacting said titaniferous materials with a high surface area carbon during the chlorination process. A process for preparing said high surface area carbon is also described.
    Type: Grant
    Filed: January 23, 1981
    Date of Patent: May 11, 1982
    Assignee: SCM Corporation
    Inventors: James P. Bonsack, Fred Schneider, Jr.
  • Patent number: 4279871
    Abstract: Vanadium impurities in chlorinated titaniferous materials are rendered easily removable by reacting said chlorinated titaniferous materials with a high surface area carbon at an elevated temperature. A process for preparing said high surface are a carbon is also described.
    Type: Grant
    Filed: June 6, 1980
    Date of Patent: July 21, 1981
    Assignee: SCM Corporation
    Inventor: James P. Bonsack
  • Patent number: 4252774
    Abstract: A method of producing aluminum chloride from aluminous materials containing compounds of iron, titanium and silicon comprising reacting the aluminous materials with carbon and a chlorine-containing gas at a temperature of about 900.degree. K. to form a gaseous mixture containing chlorides of aluminum, iron, titanium and silicon and oxides of carbon; cooling the gaseous mixture to a temperature of about 400.degree. K. or lower to condense the aluminum chlorides and iron chlorides while titanium chloride and silicon chloride remain in the gas phase to effect a separation thereof; heating the mixture of iron chlorides and aluminum chlorides to a temperature of about 800.degree. K. to form gaseous aluminum chlorides and iron chlorides; passing the heated gases into intimate contact with aluminum sulfide to precipitate solid iron sulfide and to form additional gaseous aluminum chlorides; and separating the gaseous aluminum chloride from the solid iron sulfide.
    Type: Grant
    Filed: March 25, 1980
    Date of Patent: February 24, 1981
    Assignee: The United States of America as represented by the United States Department of Energy
    Inventors: Raouf O. Loutfy, Rudolf Keller, Neng-Ping Yao
  • Patent number: 4244926
    Abstract: A process for the selective removal of iron from a ferruginous ore which comprises feeding the dried heated ore into a countercurrent reactor comprising a sulphidizing zone, an intermediate zone and a chlorination zone, through which zones the ore moves in sequence and wherein(a) in the sulphidizing zone, a reductant is introduced and the iron values present in the ore react selectively with sulphur and/or volatile sulphur-containing compounds in the presence of the reductant to form iron sulphides;(b) in the intermediate zone, volatile ferric chloride formed in the chlorinating zone is introduced and reacts with the sulphidized ore to convert the iron sulphides into ferrous chloride and reform the sulphur and/or volatile sulphur containing compounds;(c) in the chlorination zone, chlorine is introduced and converts the ferrous chloride formed in the intermediate zone into volatile ferric chloride;(d) the volatile iron chlorides and the upgraded host oxide are separately removed from the chlorination zone; and
    Type: Grant
    Filed: June 15, 1979
    Date of Patent: January 13, 1981
    Assignee: Commonwealth Scientific and Industrial Research Organization
    Inventors: Ernest Foley, Michael W. Wadsley
  • Patent number: 4083923
    Abstract: The present invention provides a process for the production of aluminum chloride and alumina of metallurgical grade purity, and valuable by-products from aluminous ores like clay, bauxites and laterites. The process comprises carbo-chlorination of the ore to produce aluminum chloride and other metal chlorides. The aluminum chloride is separated, purified and utilized as such or oxidized to make alumina while the other metal chlorides are processed to recover maximum values.
    Type: Grant
    Filed: January 22, 1976
    Date of Patent: April 11, 1978
    Assignee: Toth Aluminum Corporation
    Inventors: Alfred Lippman, Roger Frank Sebenik
  • Patent number: 4046853
    Abstract: The simultaneous chlorination of the iron and titanium values in an iron containing titaniferous ore such as ilmenite is advantageously conducted to convert the iron values to ferrous chloride but the resulting gaseous effluent is difficult to process to recover the titanium tetrachloride. The iron values in the effluent are partially oxidized according to the equation3FeCl.sub.2 + 3/4O.sub.2 .fwdarw. 1/2Fe.sub.2 O.sub.3 + 2FeCl.sub.3thereby reducing the vapor partial pressure of the ferrous chloride while maintaining the presence of some ferrous chloride to scavenge any chlorine emitted from the chlorination stage. The residual gaseous iron chlorides are condensed and chlorine-free titanium tetrachloride may be recovered from the remaining gases. If chlorine-free titanium tetrachloride is not required the mixture of gases resulting from the partial oxidation are reduced in temperature of from 500.degree. C to 800.degree.
    Type: Grant
    Filed: June 15, 1976
    Date of Patent: September 6, 1977
    Assignee: Laporte Industries Limited
    Inventor: Michael Robinson
  • Patent number: 4046854
    Abstract: The recovery of titanium tetrachloride from a mixed titanium tetrachloride/ferric chloride vapor, suitably as produced by the fluidized bed chlorination of an iron containing titaniferous ore such as ilmenite is by treating the vapor with excess oxygen over that required in theory to oxidize the ferric chloride content thereof while maintaining the vapor at a temperature within the range of 500.degree. C to 800.degree. C, removing the resulting ferric oxide particles from the vapor, cooling the vapor to a temperature above the boiling point of titanium tetrachloride to condense residual ferric chloride in the vapor and separating the condensed ferric chloride, and recovering the remaining titanium tetrachloride containing vapor.The residual ferric chloride, and chlorine remaining in the vapor after recovery of the titanium tetrachloride may be recycled.
    Type: Grant
    Filed: June 15, 1976
    Date of Patent: September 6, 1977
    Assignee: Laporte Industries Limited
    Inventor: John Dunderdale
  • Patent number: 3939244
    Abstract: Process for the purification of titanium tetrachloride, in which the said titanium tetrachloride is brought into contact with a purifying agent consisting of an inert support in granular form on which metallic sodium or other reducing metal has been deposited in sub-divided form, the said contact taking place either on crude liquid titanium tetrachloride with subsequent distillation to recover the purified titanium tetrachloride or on crude vaporised titanium tetrachloride with subsequent condensation to recover the purified titanium tetrachloride.
    Type: Grant
    Filed: November 27, 1972
    Date of Patent: February 17, 1976
    Assignee: Societa Italiana Resine S.I.R. S.p.A.
    Inventors: Luigi Piccolo, Antonio Paolinelli, Marcello Ghirga
  • Patent number: D266588
    Type: Grant
    Filed: October 15, 1979
    Date of Patent: October 19, 1982
    Assignee: Warner-Lambert Company
    Inventor: John W. Mellars