Reacting With Oxiding Gas Patents (Class 423/613)
  • Patent number: 5942201
    Abstract: The hydrolysis of carbonyl sulfide is substantially improved by utilizing titanium dioxide particles as a catalyst. It is especially favorable, if the titanium dioxide particle are sintered and treated with sodium hydroxide or sodium aluminate. Through such a treatment, the catalyst can be regenerated and reutilized.
    Type: Grant
    Filed: February 1, 1993
    Date of Patent: August 24, 1999
    Assignee: Kronos, Inc.
    Inventor: Achim Hartmann
  • Patent number: 5922120
    Abstract: The present invention provides a process for producing titanium dioxide (TiO.sub.2) pigment having a coating comprising silica and a second oxide selected from the group consisting of oxides of boron, phosphorus, magnesium, niobium, germanium, and mixtures thereof, comprising the steps of (a) reacting titanium tetrachloride (TiCl.sub.4) in the vapor phase with an aluminum compound and an oxygen-containing gas in a reactor at a temperature in the range of about 900.degree. C. to about 1600.degree. C. to provide a gaseous suspension comprising TiO.sub.2 particles, (b) contacting the gaseous suspension comprising the TiO.sub.2 particles with a silicon halide and an oxide precursor of boron, phosphorus, magnesium, niobium, germanium, and mixtures thereof, and (c) cooling the gaseous suspension to produce TiO.sub.2 pigment having a coating comprising silica and a second oxide.
    Type: Grant
    Filed: December 23, 1997
    Date of Patent: July 13, 1999
    Assignee: E. I. du Pont de Nemours and Company
    Inventors: Narayanan Sankara Subramanian, Pratibha Laxman Gai, Russell Bertrum Diemer, Jr., Alvin Allen, John Steven Gergely
  • Patent number: 5861132
    Abstract: A gas phase process for the production of titanium dioxide powders having well-controlled crystalline and surface area characteristics is disclosed. In this process, which is preferably carried out in a laminar diffusion flame reactor, vapor phase TiCl.sub.4 and oxygen are mixed in a reaction area which is heated externally. The titanium dioxide powder formed is then collected. It is preferred that the heat source used be a hydrocarbon fueled (e.g., methane) flame. Optionally, a vapor phase dopant (such as SiCl.sub.4) may be added to the reaction mixture to desirably affect the physical properties of the titanium dioxide produced. In a particularly preferred embodiment, a corona electric field is positioned across the area where the combustion reaction takes place (i.e., the reaction area). High anatase, high surface area titanium dioxide powders made by this process are excellent photocatalysts. The products of this process and the use of those products as photocatalysts are also disclosed.
    Type: Grant
    Filed: September 4, 1997
    Date of Patent: January 19, 1999
    Assignee: University of Cincinnati
    Inventors: Sotiris Emmanuel Pratsinis, Srinivas Vemury, George P. Fotou, Andreas Gutsch
  • Patent number: 5840112
    Abstract: A process for reacting titanium tetrachloride vapors with oxygen including a first oxygen preheat assembly for preheating oxygen to a first predetermined temperature and a titanium tetrachloride preheat assembly for preheating titanium tetrachloride to a relatively low, temperature. The process includes adding a second oxygen preheat assembly for preheating oxygen to a second temperature substantially below the first temperature, and includes a second reaction zone adapted for receiving the mixture from the first reaction zone, the oxygen at the second temperature being reacted with the titanium tetrachloride in the mixture from the first reaction zone to produce titanium dioxide. Also provided is a process for the preparation of titanium dioxide comprising reacting titanium tetrachloride with oxygen at an elevated pressure and at a temperature above about 1750.degree. F.
    Type: Grant
    Filed: July 25, 1996
    Date of Patent: November 24, 1998
    Assignee: Kerr McGee Chemical Corporation
    Inventors: A. J. Morris, J. C. Magyar, G. D. Wootten, W. A. Yuill
  • Patent number: 5759511
    Abstract: This invention relates to an improved process for making titanium dioxide pigment, wherein granular scouring particles (scrubs) comprising specific water-soluble salts (KCl, CsCl, or mixtures thereof) are introduced into a cooling conduit containing a hot gaseous suspension of titanium dioxide particulate. The process provides titanium dioxide pigment having higher carbon black undertone (CBU) levels.
    Type: Grant
    Filed: August 26, 1996
    Date of Patent: June 2, 1998
    Assignee: E. I. du Pont de Nemours and Company
    Inventors: Russell Bertrum Diemer, Jr., Narayanan Sankara Subramanian, David A. Zimmerman
  • Patent number: 5749937
    Abstract: A fast quench reaction includes a reactor chamber having a high temperature heating means such as a plasma torch at its inlet and a restrictive convergent-divergent nozzle at its outlet end. Reactants are injected into the reactor chamber. The resulting heated gaseous stream is then rapidly cooled by passage through the nozzle. This "freezes" the desired end product(s) in the heated equilibrium reaction stage.
    Type: Grant
    Filed: March 14, 1995
    Date of Patent: May 12, 1998
    Assignee: Lockheed Idaho Technologies Company
    Inventors: Brent A. Detering, Alan D. Donaldson, James R. Fincke, Peter C. Kong
  • Patent number: 5728205
    Abstract: The present invention provides a process for producing titanium dioxide (TiO.sub.2) pigment comprising boron oxide (B.sub.2 O.sub.3), comprising the steps of: (a) reacting titanium tetrachloride (TiCl.sub.4) in the vapor phase with an aluminum compound and an oxygen-containing gas in a reactor at a temperature in the range of about 900.degree. C. to about 1600.degree. C. to provide a gaseous suspension comprising TiO.sub.2 particles, and (b) contacting the gaseous suspension comprising the TiO.sub.2 particles with a boron compound to produce TiO.sub.2 pigment comprising B.sub.2 O.sub.3.
    Type: Grant
    Filed: December 11, 1996
    Date of Patent: March 17, 1998
    Assignee: E. I. du Pont de Nemours and Company
    Inventors: Alvin Allen, John Steven Gergely
  • Patent number: 5698177
    Abstract: A gas phase process for the production of titanium dioxide powders having well-controlled crystalline and surface area characteristics is disclosed. In this process, which is preferably carried out in a laminar diffusion flame reactor, vapor phase TiCl.sub.4 and oxygen are mixed in a reaction area which is heated externally. The titanium dioxide powder formed is then collected. It is preferred that the heat source used be a hydrocarbon fueled (e.g., methane) flame. Optionally, a vapor phase dopant (such as SiCl.sub.4) may be added to the reaction mixture to desirably affect the physical properties of the titanium dioxide produced. In a particularly preferred embodiment, a corona electric field is positioned across the area where the combustion reaction takes place (i.e., the reaction area). High anatase, high surface area titanium dioxide powders made by this process are excellent photocatalysts. The products of this process and the use of those products as photocatalysts are also disclosed.
    Type: Grant
    Filed: June 8, 1995
    Date of Patent: December 16, 1997
    Assignees: University of Cincinnati, Universitat Karlsruhe
    Inventors: Sotiris Emmanuel Pratsinis, Srinivas Vemury, George P. Fotou, Andreas Gutsch
  • Patent number: 5651864
    Abstract: A method for synthesizing a particulate product including electrostatically charging a fuel and/or oxidizer and/or ionizable inert gas present during the synthesis is provided. The method can include a step of collecting the particulate product which exploits the charged nature of the particulate reaction product.
    Type: Grant
    Filed: February 27, 1996
    Date of Patent: July 29, 1997
    Assignee: Kerr-McGee Corporation
    Inventor: Phillip M. Story
  • Patent number: 5618580
    Abstract: The present invention provides a method for producing ceramic fine particles comprising the steps of supplying gaseous starting materials or starting material droplets to a reaction space arranged in an annular portion between inner and outer cylinders of a coaxial, double-cylinder reaction apparatus, the reaction apparatus having a stationary outer cylinder and a rotatable inner cylinder; and subjecting the gaseous starting materials or the starting material droplets to reaction in the reaction space while rotating the inner cylinder. Also, the present invention provides a production apparatus used therefor.
    Type: Grant
    Filed: June 15, 1995
    Date of Patent: April 8, 1997
    Assignee: Kao Corporation
    Inventors: Kentaro Oshima, Toshiharu Numata, Toru Nishimura, Sachiko Kokubo, Keiichi Tsuto
  • Patent number: 5607648
    Abstract: A rotary kiln, particularly for producing uranium dioxide from uranium hexafluoride, has an inlet arrangement and a heated rotatable barrel. Uranium hexafluoride and steam react together in the inlet arrangement to form uranyl fluoride which is fed into the barrel by the aid of a rotating scroll feed device. In the barrel, the uranyl fluoride reacts with a counterflow stream of steam and hydrogen to produce the uranium dioxide. A porous metal or ceramic filter closely surrounds the scroll feed device to remove particles from kiln-produced gases. The filter is maintained in a clean condition by the scraping action of a number of helical blades forming part of the scroll feed device. The uranium dioxide powder produced by the kiln may be processed to form nuclear fuel pellets.
    Type: Grant
    Filed: January 20, 1995
    Date of Patent: March 4, 1997
    Assignee: British Nuclear Fuels plc
    Inventors: Robert Carter, John T. Semeraz
  • Patent number: 5599519
    Abstract: A novel process for the preparation of titanium dioxide comprises reacting titanium tetrachloride with oxygen at an elevated pressure and a temperature above 700.degree. C. The titanium tetrachloride is introduced into the reactor in at least two points and that portion introduced in the first inlet point is admixed with aluminium chloride and has been heated to a temperature of at least 450.degree. C. by utilizing the heat of reaction of aluminium and chlorine. The process provides an energy efficient method for producing titanium dioxide and avoids the need for auxiliary heating of the reactor by, for example, hydrocarbon combustion or electric discharge, which auxiliary heating can introduce impurities into the product titanium dioxide.
    Type: Grant
    Filed: March 27, 1995
    Date of Patent: February 4, 1997
    Assignee: Tioxide Group Services Limited
    Inventor: Andrew J. Haddow
  • Patent number: 5573744
    Abstract: A method and apparatus for producing TiO.sub.2 by reacting O.sub.2 and TiCl.sub.4 in a reactor tube wherein pressure fluctuations in the flow of fluids through the reactor tube are sensed and output signals are generated proportional to the sensed pressure fluctuations. The flow of at least one of the TiCl.sub.4 or O.sub.2 is then varied through the reactor tube in response to predetermined pressure fluctuations so as to increase the efficiency of the reaction between TiCl.sub.4 and the O.sub.2. The efficiency of the reaction between O.sub.2 and TiCl.sub.4 in the reactor tube is achieved by a control apparatus operably connected to the reactor assembly which is capable of monitoring pressure fluctuations in TCl.sub.4 and O.sub.2 through the reactor assembly so that the flow of at least one of the TiCl.sub.4 or O.sub.2 can be varied in response to predetermined pressure fluctuations. The control apparatus includes a sensor assembly, a signal conditioning unit and a signal processing unit.
    Type: Grant
    Filed: February 17, 1995
    Date of Patent: November 12, 1996
    Assignee: Kerr-McGee Corporation
    Inventors: Vernon D. Gebben, Walter D. Bruce
  • Patent number: 5562764
    Abstract: A process for producing substantially anatase-free TiO.sub.2 by addition of a silicon halide in a reaction of TiCl.sub.4 and an oxygen-containing gas in a plug flow reactor is disclosed. Pigmentary properties such as gloss and CBU are enhanced without loss of durability.
    Type: Grant
    Filed: June 23, 1995
    Date of Patent: October 8, 1996
    Assignee: E. I. du Pont de Nemours and Company
    Inventor: Raul A. Gonzalez
  • Patent number: 5556600
    Abstract: A method and apparatus for producing TiO.sub.2 by reacting O.sub.2 and TICl.sub.4 in a reactor tube wherein pressure fluctuations in the flow of fluids through the reactor tube are sensed and output signals are generated proportional to the sensed pressure fluctuations. The flow of at least one of the TiCl.sub.4 or O.sub.2 is then varied through the reactor tube in response to predetermined pressure fluctuations so as to increase the efficiency of the reaction between TiCl.sub.4 and the O.sub.2. The efficiency of the reaction between O.sub.2 and TiCl.sub.4 in the reactor tube is achieved by a control apparatus operably connected to the reactor assembly which is capable of monitoring pressure fluctuations in TCl.sub.4 and O.sub.2 through the reactor assembly so that the flow of at least one of the TiCl.sub.4 or O.sub.2 can be varied in response to predetermined pressure fluctuations. The control apparatus includes a sensor assembly, a signal conditioning unit and a signal processing unit.
    Type: Grant
    Filed: May 26, 1995
    Date of Patent: September 17, 1996
    Assignee: Kerr-McGee Chemical Corporation
    Inventors: Vernon D. Gebben, Walter D. Bruce
  • Patent number: 5538708
    Abstract: In the process for producing titanium dioxide by (a) reacting titanium tetrachloride and oxygen in the vapor phase in a reactor to produce titanium dioxide, and (b) subsequently cooling the titanium dioxide by passing it through a flue consisting of a conventional flue, a finned flue, or combinations thereof, wherein the outlet for the reactor in step (a) has a smaller interior diameter than the inlet for the flue in step (b),the improvement comprising passing the titanium dioxide through a truncated cone-shaped finned flue conduit, the smaller diameter end of the truncated cone-shaped finned flue conduit receiving titanium dioxide produced by the reactor and the larger diameter end of the truncated cone-shaped finned flue conduit discharging titanium dioxide that is received by the flue.
    Type: Grant
    Filed: December 6, 1994
    Date of Patent: July 23, 1996
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Raul A. Gonzalez, Charles D. Musick
  • Patent number: 5536487
    Abstract: Small quantities of an alkali metal salt control additive, along with the addition of a rutile promotion additive, preferably aluminum trichloride as ruffle promoter, is added in the oxidation of titanium tetrachloride into the titanium dioxide burner reaction zone. Metal used to make aluminum trichloride is introduced into a aluminum chloride generator reactor in a main branch, and the alkali metal salt is introduced in a subsidiary branch in a controlled addition provided by a "dilution" mixture of the salt in aluminum powder and preferably by applying additional agents which improve the flee-flowing properties of the mixture such as, for example, anhydrous potassium oleate.
    Type: Grant
    Filed: February 27, 1995
    Date of Patent: July 16, 1996
    Assignee: Kronos, Inc.
    Inventor: Achim Hartmann
  • Patent number: 5508015
    Abstract: A chloride process for producing TiO.sub.2 by addition of an inert gas in a vapor phase reaction of TiCl.sub.4 and an oxygen-containing gas is disclosed.
    Type: Grant
    Filed: July 15, 1994
    Date of Patent: April 16, 1996
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Raul A. Gonzalez, Charles D. Musick, James N. Tilton
  • 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: 5300273
    Abstract: An improved process is provided for producing titanium tetrachloride vapor admixed with a desired particular amount of aluminum trichloride vapor for use in the production of rutile titanium dioxide. The vapor mixture is derived from a titanium tetrachloride solution containing the desired particular amount of aluminum trichloride. The solution is produced continuously by dissolving aluminum trichloride in a heated stream of liquid titanium tetrachloride utilizing a cyclic aluminum trichloride bed switching and recharging process.
    Type: Grant
    Filed: December 3, 1992
    Date of Patent: April 5, 1994
    Assignee: Kerr-McGee Chemical Corporation
    Inventor: Robert E. Leonard
  • 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: 5204083
    Abstract: An improved method for preparing a rutile titanium dioxide pigment of uniform particle size wherein the pigment is formed by reaction of a mixture of an oxidizing gas and a titanium halide in the vapor phase at elevated temperatures in the presence of a metal ion containing compound. The improvement comprises introducing the metal ion containing compound into a vapor phase oxidation reactor containing the reacting mixture in at least two separate and discrete increments. The first increment is introduced into the reactor at a point prior to reaction of said mixture having occurred while the second increment is introduced into the reactor at a point wherein at least 20 weight percent of the total titanium halide reactant has been converted to the desired titanium dioxide pigment.
    Type: Grant
    Filed: May 23, 1988
    Date of Patent: April 20, 1993
    Assignee: Kerr-McGee Chemical Corporation
    Inventors: John C. Magyar, R. Gerald McDill, Eugene R. Adams
  • Patent number: 5201949
    Abstract: Titanium dioxide pigment prepared by the high pressure (e.g., 10-200 PSIG) oxidation of TiCl.sub.4 vapor is improved with respect to carbon black undertone, specific surface area, and gloss properties by the addition of a nucleant consisting essentially of a cesium substance which is present in the amount of about 8-2,000 parts per million, based on the weight of the TiO.sub.2. The foregoing process is also used wherein the residence time of the reactants in the mixing zone of the reactor is about 1-16 milliseconds.
    Type: Grant
    Filed: May 20, 1992
    Date of Patent: April 13, 1993
    Assignee: E. I. du Pont de Nemours and Company
    Inventors: Alvin Allen, Glenn R. Evers
  • Patent number: 5196181
    Abstract: A process for the production of titanium dioxide through the reaction of vaporous TiCl.sub.4 with oxygen under a pressure of between 2.4 and 3.4 bar, and a corresponding apparatus are used to achieve long permanent operation times. The oxygen required is indirectly preheated to between 850.degree. and 1000.degree. C. In a reaction chamber closed at one end, configured inside for advantageous flow and lined at least partly with refractories, the indirectly preheated oxygen is further heated by direct contact with very hot combustion gases of an auxiliary flame to temperatures, as is required, for the spontaneous reaction with the TiCl.sub.4 introduced downstream into the reaction chamber.
    Type: Grant
    Filed: November 7, 1990
    Date of Patent: March 23, 1993
    Assignee: Kronos (USA), Inc.
    Inventor: Achim Hartmann
  • Patent number: 4937062
    Abstract: The present invention includes metal oxide foam particles and a method of making the same. A decomposable metal salt feed solution is injected into a hot atomizing gas. The mixture of hot atomizing gas and feed solution is maintained in the reactor until the feed solution converts to metal oxide foam particles. The metal oxide foam particles have a high specific surface area.
    Type: Grant
    Filed: March 7, 1988
    Date of Patent: June 26, 1990
    Assignee: Cabot Corporation
    Inventors: Merrill Jordan, deceased, Steven R. Reznek, Matthew Neville, Brian A. Soucy, Bruce E. Mackay
  • Patent number: 4937064
    Abstract: In the process for producing titanium dioxide by(a) reacting titanium tetrachloride and oxygen in the vapor phase to produce titanium dioxide, and(b) subsequently cooling the titanium dioxide in a flue,an improvement comprising utilizing for all or a portion of the flue a conduit having a plurality of internal, substantially longitudinal protuberances, depressions or both.
    Type: Grant
    Filed: September 29, 1988
    Date of Patent: June 26, 1990
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Raul A. Gonzalez
  • Patent number: 4803056
    Abstract: A system for increasing the capacity of a process for producing titanium dioxide by reacting titanium tetrachloride vapors with oxygen wherein the process includes an oxygen preheat assembly for preheating oxygen to a predetermined temperature level and a first titanium tetrachloride preheat assembly for preheating titanium tetrachloride to a first, relatively high, temperature level, a portion of the oxygen and the titanium tetrachloride vapors at the first temperature level being reacted in a first reaction zone to produce a mixture of titanium dioxide reaction product, oxygen and unreacted titanium tetrachloride vapors at the first temperature level.
    Type: Grant
    Filed: July 31, 1985
    Date of Patent: February 7, 1989
    Assignee: Kerr-McGee Chemical Corporation
    Inventors: Alan J. Morris, Merlin D. Coe
  • Patent number: 4797163
    Abstract: Energy required for the calcining or drying operations in the production of titanium dioxide by the sulfate process and the chloride process is at least in part provided by burning by-product offgases containing carbon monoxide obtained in the chlorination of titanium-containing raw materials under reducing conditions.
    Type: Grant
    Filed: August 24, 1987
    Date of Patent: January 10, 1989
    Assignee: Bayer Akteingesellschaft
    Inventors: Gunter Lailach, Karl-Heinz Schultz
  • Patent number: 4784841
    Abstract: A process for the production of coarse scrubbing aggregates of TiO.sub.2 particles by vapor phase oxidation of titanium tetrachloride. The particle aggregates of sizes above 0.15 mm are separated from the TiO.sub.2 fines by wet screening on a moving screen, calcined and returned to the process. In a preferred embodiment of the process, the titanium dioxide prior to calcination is admixed with 0.01 to 0.3% by weight alkaline hydroxides (related to anhydrous TiO.sub.2), hard particle aggregates of sizes between 0.2 to 2.0 mm being generated that are returned to the hot reaction mixture and used for the prevention of deposit formation on the surfaces of the heat exchanger.The process can be carried through in such a way that the quantities of coarse scrubbing TiO.sub.2 aggregates per unit of time consumed by abrasion and newly formed by sintering are equal, their percentages in recycling TiO.sub.2 thus remaining constant which simplifies the TiO.sub.2 production process.
    Type: Grant
    Filed: September 21, 1987
    Date of Patent: November 15, 1988
    Assignee: Kronos Titan, GmbH
    Inventors: Achim Hartmann, Hans Thumm
  • Patent number: 4759800
    Abstract: A process for the improvement of titanium dioxide pigments by a post-treatment, wherein the titanium dioxide pigment produced by any process, in the form of an aqueous suspension and in any order, is treated with an aqueous titanium oxide chloride solution resulting from the scrubbing of off-gases derived from the production of titanium tetrachloride and, optionally, with one or more other water-soluble metal salts which when neutralized form difficult-to-dissolve oxide hydrates and/or other difficult-to-dissolve compounds, and/or optionally with a water-soluble silicate, and where difficult-to-dissolve oxide hydrates and/or other difficult-to-dissolve compounds are precipitated onto the titanium dioxide pigment from the titanium oxide chloride solution and, if present, from the other metal salts and/or the silicate, and where the titanium dioxide pigment thus treated is recovered such as by being separated from the suspension, washed, dried and milled.
    Type: Grant
    Filed: February 25, 1987
    Date of Patent: July 26, 1988
    Assignee: Kronos Titan, GmbH
    Inventors: Hans H. Luginsland, Franz Rosendahl
  • Patent number: 4746638
    Abstract: Alumina-titania composite powder comprising spherical particles each of which contains about 30 to 80 wt % of .gamma.- phase or .delta.-phase alumina and about 70 to 20 wt % of titania comprising rutile-phase in the majority and is substantially free from X-phase (3Al.sub.2 O.sub.3 -TiO.sub.2) and aluminum titanate-phase. These alumina-titania composite powders are prepared by blowing a vapor mixture of AlCl.sub.3 and TiCl.sub.4 into a burning flame to effect oxidation, which is characterized in that a temperature of a mixing section, where a combustible gas, an oxidizing gas, AlCl.sub.3 gas, TiCl.sub.4 gas and a carrier gas are mixed and subjected to combustion, is kept at about 1450.degree. C. or higher and lower than a melting point of aluminum titanate; a temperature of an outlet portion of a reacting section connected to the mixing section is kept at about 800.degree. C. or higher; and an average total gas retention time in the mixing section and the reacting section are 20 to 500 msec.
    Type: Grant
    Filed: September 26, 1986
    Date of Patent: May 24, 1988
    Assignee: Kureha Chemical Industry Co., Ltd.
    Inventors: Saburo Hori, Yoshio Ishii
  • Patent number: 4578090
    Abstract: In the manufacture of particulated metal oxides by the vapor phase oxidation of volatile metal halides, hot gaseous effluent streams are produced which, after separation of the desired particulated metal oxide therefrom, contain residual amounts of the particulated metal oxide as well as unreacted, volatile metal halide and halogen gas. The method of this invention provides for the recovery of these materials, individually, through a succession of contacting and separating steps utilizing a recycle stream of previously recovered, unreacted, liquid metal halide. Utilization of the recycle stream of metal halide provides for both evaporative cooling of the hot gaseous effluent stream to permit recovery of the residual particulated metal oxide therein and scrubbing of the resulting off-gas to recover the unreacted volatile metal halide therein as a liquid and provide a gas phase containing the by-product halogen gas.
    Type: Grant
    Filed: October 15, 1984
    Date of Patent: March 25, 1986
    Assignee: Kerr-McGee Chemical Corporation
    Inventor: Theodore A. Rado
  • Patent number: 4515762
    Abstract: Waste gases resulting from the production of silicon in connection with the ormation or decomposition of chlorosilanes, which gases always contain hydrogen chloride, can be worked up without removal of the hydrogen chloride. For this purpose, the waste gases which, after separation from the chlorosilanes, only contain hydrogen and hydrogen chloride, are subjected to combustion with addition of air and, after addition of silicon tetrachloride, the result being highly dispersed SiO.sub.2. The hydrogen chloride then remaining in the gaseous phase is returned to the process stream for production of trichlorosilane.
    Type: Grant
    Filed: November 16, 1982
    Date of Patent: May 7, 1985
    Assignee: Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe mbH
    Inventors: Rudolf Griesshammer, Franz Koppl, Winfried Lang, Ernst Muhlhofer, Michael Schwab
  • Patent number: 4462979
    Abstract: A flue for cooling the flow of reaction product from the high temperature oxidation of a metal halide to the metal oxide in the presence of oxygen, said flue comprising a first section wherein the cross-sectional area is increased thereby decreasing the turbulence of the flow and a second section wherein the cross-sectional area is decreased thereby increasing the velocity or turbulence of the flow and the process for using said flue to produce an agglomerate of TiO.sub.2 particles that are readily filterable and easily ground.
    Type: Grant
    Filed: February 25, 1982
    Date of Patent: July 31, 1984
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Joel B. Hill, Jr., William E. Stevens, Reg Davies
  • Patent number: 4455288
    Abstract: In a process for the production of titanium dioxide by the vapour phase oxidation of titanium tetrachloride in which process entrained inert particulate material is passed through equipment used to reduce or prevent the deposition of solids thereon, the quantity of inert particulate material entrained may be affected by the varying back pressure normally obtaining in the equipment. The control of this quantity may be improved by reducing pressure differences (by means of conduit 39) between the inlet (40) and outlet (36) of a mechanical feeding device (29, 30) for the solids. This entails the transmission of the pressure (from the conduit 26) into the solids delivery system 25(17) and this may be alleviated, optionally, by maintaining a head of solids in the system and/or by using a system of pressurized hoppers. The invention enables the quantity of inert particulate material used to be reduced.
    Type: Grant
    Filed: November 20, 1981
    Date of Patent: June 19, 1984
    Assignee: Laporte Industries Limited
    Inventors: David Salter, David Scott
  • Patent number: 4426550
    Abstract: An improved multiwire conductor of the type which is mechanically stabilized by a tin based solder filler. A solder filled conductor is heated to a temperature above its melting point for a period long enough to allow a substantial amount of copper to be dissolved from the wires comprising the conductor. The copper forms the brittle intermetallic compound Cu.sub.5 Sn.sub.6 with tin in the solder. After cooling the conductor is flexed causing a random cracking of the solder, and thereby increasing the interwire resistance of the conductor. The subject invention is particularly adapted for use with braided, ribbon-type solder filled superconductors.
    Type: Grant
    Filed: March 15, 1982
    Date of Patent: January 17, 1984
    Assignee: The United States of America as represented by the United States Department of Energy
    Inventors: Thomas Luhman, Masaki Suenaga
  • Patent number: 4389391
    Abstract: An improved method of beneficiating ilmenite using two chlorinators in order to oxidize by-product iron chlorides to chlorine in the vapor phase and eliminate the necessity of separating the chlorine from combustion gas by cryogenic methods comprising using a first stage which produces beneficiated ore, and, inter alia, carbon dioxide, iron chlorides, predominantly ferrous chloride, which are condensed to gain the separation from CO.sub.2 ; solid iron chlorides are fed to an oxidation zone in the void above the second stage beneficiator and reacted with oxygen; heat required for vaporization of the condensed chlorides is supplied in part by beneficiation within the second stage. The fluidized bed overflow of the second stage beneficiator is magnetically separated to separate practically pure T.sub.1 O.sub.2, useful as a starting material for T.sub.1 O.sub.2 pigment and a recycle stream of magnetic partially beneficiated ore.
    Type: Grant
    Filed: June 28, 1981
    Date of Patent: June 21, 1983
    Inventor: Wendell E. Dunn, Jr.
  • Patent number: 4355015
    Abstract: The residual gas obtained in the pyrogenic production of metal oxides or metalloid oxides contain besides the desired product elemental chlorine if a chlorine containing starting material is employed. After cooling the residual gas the elemental chlorine is reacted to form hydrogen chloride by using an aqueous solution of a reducing agent and in this form the chlorine is subsequently washed out of the residual gas.
    Type: Grant
    Filed: June 6, 1980
    Date of Patent: October 19, 1982
    Assignee: Degussa Aktiengesellschaft
    Inventors: Emil Heckel, Freddy Seys, Rene Baeckelmans, Wolfgang Heilmann
  • Patent number: 4347229
    Abstract: There is provided a pyrogenic process for the production of finely divided oxide of a metal and/or a metalloid in which there is employed as the starting material a vaporizable halogen compound of a metal and/or metalloid. Because of the starting material there is formed elemental halogen which is an impurity in the oxide formed. To remove the halogen there is supplied to the cooling section of the production plant a mixture of hydrogen and inert gas.
    Type: Grant
    Filed: June 3, 1980
    Date of Patent: August 31, 1982
    Assignee: Degussa Aktiengesellschaft
    Inventors: Josef Schmid, Ludwig Lange, Hans Klebe, Dieter Schutte
  • Patent number: 4258023
    Abstract: In case of the pyrogenous production of metal oxides or metalloid oxides, whenever a halogen compound is used as a starting material, an elementary halogen is formed as a byproduct. This may be converted in the cooling section of the reaction apparatus with hydrogen into hydrogen halide.For a better temperature control and prevention of uncontrolled deflagration of the hydrogen in case of the halogen detonating gas reaction, according to the invention the hydrogen is introduced into the cooling section by means of a double jacket pipe, whereby an inert gas is introduced additionally by way of the interstice between the inside wall and the outside jacket of the double jacket pipe into the cooling section.
    Type: Grant
    Filed: October 16, 1979
    Date of Patent: March 24, 1981
    Assignee: Deutsche Gold-und Silber-Scheideanstalt Vormals Roessler
    Inventors: Josef Schmid, Ludwig Lange, Hans Klebe, Dieter Schutte
  • Patent number: 4241042
    Abstract: Titanium dioxide, in the form of discrete, solid substantially spherical particles of a substantially uniform shape and size, is obtained by providing an aerosol comprising discrete liquid particles of a hydrolyzable titanium compound, contacting the aerosol with water vapor in dynamic flow to hydrolyze the liquid titanium (IV) compound to titanium dioxide, and recovering the desired product.
    Type: Grant
    Filed: June 19, 1978
    Date of Patent: December 23, 1980
    Assignee: Montedison S.p.A.
    Inventors: Egon Matijevic, Mario Visca
  • Patent number: 4214913
    Abstract: A process for preparing rutile TiO.sub.2 by a process comprising oxidizing with oxygen or an oxygen containing gas, a mixture TiCl.sub.4 and AlCl.sub.3 and after at least 80% of the TiCl.sub.4 has been converted to TiO.sub.2 adding sufficient PCl.sub.3 to form from 0.1-0.5% P.sub.2 O.sub.5 in the TiO.sub.2, the amount of AlCl.sub.3 being sufficient to form 0.1-1.5% Al.sub.2 O.sub.3 in the TiO.sub.2.
    Type: Grant
    Filed: March 5, 1979
    Date of Patent: July 29, 1980
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Hans H. Glaeser
  • Patent number: 4170630
    Abstract: This invention relates to a process and apparatus for producing particulate solids from vaporous reactants in a reactor wherein the reactor zone is remote from the feed inlets to the reactor.
    Type: Grant
    Filed: June 13, 1974
    Date of Patent: October 9, 1979
    Assignee: American Cyanamid Company
    Inventor: Harold E. Hoelscher
  • Patent number: 4145403
    Abstract: An arc heater method and system for producing a high energy source characterized by a housing forming a mixing compartment, a plurality of arc heaters radially mounted on the housing and communicating with the mixing compartment, a reactor communicating with the downstream end of the mixing compartment with a reduced opening therebetween, inlet means at the downstream end of the compartment for introducing an oxidizable metal compound into the reactor, and means within the mixing compartment for flowing superheated gases from the arc heaters at the upstream end of the compartment and into the reactor.
    Type: Grant
    Filed: September 29, 1977
    Date of Patent: March 20, 1979
    Inventors: Maurice G. Fey, Charles B. Wolf
  • Patent number: 4120941
    Abstract: Process of oxidizing halides, including mixtures thereof, with oxygen, oxygen-containing gases and/or oxygen-liberating substances in a combustion chamber, whereby the vapor pressure of the halides at introduction to the combustion or oxidation chamber is greater than the pressure within the combustion chamber. Recovery of halides at greater purity with substantial decrease of by-product deposits on operating equipment is realized.
    Type: Grant
    Filed: October 31, 1974
    Date of Patent: October 17, 1978
    Assignee: Halomet AG
    Inventors: Rudolf Nowak, Gerhard Holland
  • Patent number: 4097301
    Abstract: Process for producing aqueous slurries of chloride process anatase titanium dioxide pigment by adding to the slurry from 0.03 to 0.45% by weight of sodium aluminate or aluminum trichloride, calculated as Al.sub.2 O.sub.3 and based on the weight of the titanium dioxide pigment. The resulting slurries retain relatively low viscosity for at least one day.
    Type: Grant
    Filed: March 30, 1977
    Date of Patent: June 27, 1978
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Hans-Achim Dietmar Wildt
  • Patent number: 4083946
    Abstract: A process for removing chloride impurities from TiO.sub.2 by injecting a gas selected from steam, air, nitrogen, or a mixture thereof, at a sonic or a supersonic velocity, a pressure of about 25-600 psi, and a temperature of about 140.degree.-650.degree. C., into the TiO.sub.2 to disperse it, and then separating the TiO.sub.2 from the gas and chlorides.
    Type: Grant
    Filed: March 23, 1977
    Date of Patent: April 11, 1978
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: George Alan Schurr, Hans-Achim Dietmar Wildt
  • Patent number: 4053577
    Abstract: Process and apparatus for the production of finely-divided metal oxides by the oxidation of the corresponding metal halide wherein a secondary gas is introduced into a heated primary gas through apertures in the reaction zone wall, the apertures formed with at least two different cross-sectional areas along their length, the small cross-sectional area being at the inlet end of the aperture for the secondary gas.
    Type: Grant
    Filed: August 11, 1975
    Date of Patent: October 11, 1977
    Assignee: Tioxide Group Limited
    Inventor: Kenneth Arkless
  • Patent number: 4013782
    Abstract: Apparatus and process suitable for oxidising a metal halide in the vapor phase wherein at least part of the wall of the reaction zone is formed from crimped annular plates separated by uncrimped annular plates to form orifices through which at least one of the reactants can be introduced into the reaction zone.
    Type: Grant
    Filed: February 13, 1974
    Date of Patent: March 22, 1977
    Assignee: Tioxide Group Limited
    Inventors: Stanley Powell, Glyn Thomas
  • Patent number: 4012201
    Abstract: Apparatus suitable for oxidizing a metal halide in the vapor phase wherein at least part of the wall of the reaction zone is formed from crimped annular plates separated by uncrimped annular plates to form orifices through which at least one of the reactants can be introduced into the reaction zone.
    Type: Grant
    Filed: October 23, 1974
    Date of Patent: March 15, 1977
    Assignee: Tioxide Group Limited
    Inventors: Stanley Powell, Glyn Thomas