Anhydrous Magnesium Chloride Patents (Class 423/498)
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Patent number: 11261467Abstract: A method for conversion of magnesium chloride into magnesium oxide and HCl, comprising the steps of providing a magnesium chloride compound to a thermohydrolysis reactor, the reactor being at a temperature of at least 300° C., withdrawing MgO from the thermohydrolysis reactor in solid form, and withdrawing a HCl containing gas stream from the thermohydrolysis reactor, wherein the magnesium chloride compound provided to the thermohydrolysis reactor is a solid magnesium chloride compound which comprises at least 50 wt. % of MgCl2.4H2O. The process accordingly is fast and can be operated in a manner which is efficient both as regards apparatus and energy. It can also be integrated in a process for converting a magnesium chloride solution.Type: GrantFiled: March 30, 2015Date of Patent: March 1, 2022Assignee: PURAC BIOCHEM B.V.Inventors: André Banier De Haan, Jeroen Bokhove, Fesia Lestari Laksmana
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Publication number: 20140308197Abstract: A unique production of titanium compounds and metal by sustainable methods using iron-titanium oxide starting material such as ilmenite, leucoxene, or rutile is described. Here the iron-titanium oxide compound is prepared by converting the iron portion of the compound to ferrous chloride at low temperatures by using close to stoichiometric amounts of sulfur and chlorine required for all the iron oxides and the other non-titanium oxides. The ferrous chloride thus formed is removed recovering a marketable product of ferrous chloride and the ‘sustainable’ titanium oxide starting material by additional process steps. This can be converted to ‘sustainable’ titanium metal, or titanium tetra-chloride by process shown herein for further conversions to titanium dioxide pigment by present chloride process or supplied to existing titanium sponge producers, benefitting them in having a ‘sustainable process’.Type: ApplicationFiled: April 16, 2013Publication date: October 16, 2014Inventor: Indra Neelameggham
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Patent number: 8765014Abstract: Disclosed herein is a quantum dot ink composition for inkjet printing. The quantum dot ink composition comprises a highly viscous polymeric additive. Quantum dots can be ejected by inkjet printing and the concentration of the quantum dots in the quantum dot ink composition can be freely controlled. In addition, the loading amount of the quantum dots can be reduced. Based on these advantages, the quantum dot ink composition can be used as a material for light-emitting layers of a variety of electronic devices. Also disclosed herein is an electronic device fabricated using the quantum dot ink composition.Type: GrantFiled: April 25, 2008Date of Patent: July 1, 2014Assignee: Samsung Electronics Co., Ltd.Inventors: Kyung Sang Cho, Tae Woon Cha
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Publication number: 20140148372Abstract: Acidic viscoelastic cleaning compositions are disclosed which use non polymer thickening agents. According to the invention, cleaning compositions have been developed using viscoelastic surfactants in acidic cleaning formulations. These provide the dual benefit of thickening as well as an additional cleaning, thereby improving performance. Applicants have also identified several pseudo linking agents which when, used with viscoelastic surfactants provide enhanced viscoelasticity and cleaning.Type: ApplicationFiled: November 28, 2012Publication date: May 29, 2014Applicant: ECOLAB USA INC.Inventors: Victor Fuk-Pong Man, Michael Charles Denoma, Yvonne Marie Killeen, Susan Maloney Viall
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Patent number: 8377409Abstract: Methods for making brines may generally comprise forming a mixture comprising: (i) a solid material produced as a by-product of the Kroll process including solid anhydrous magnesium chloride and solid elemental magnesium; (ii) an amount of a previously-produced brine; and (iii) an amount of water sufficient to provide a predetermined brine concentration. At least a portion of the solid material in the mixture is dissolved while simultaneously controlling the temperature of the mixture. At least a portion of insoluble matter is separated from the mixture.Type: GrantFiled: September 15, 2009Date of Patent: February 19, 2013Assignee: ATI Properties, Inc.Inventor: James A. Sommers
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Publication number: 20110104042Abstract: A unique method of convective dissolution of salts from in situ ponds by trenching salt beds, introducing dissolution waters to promote convective dissolution, pumping out the saturated solution from the pond bottom, and introducing additional dissolution waters.Type: ApplicationFiled: January 5, 2011Publication date: May 5, 2011Inventor: Abraham Sadan
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Publication number: 20110085963Abstract: A unique method of convective dissolution of salts from in situ ponds by trenching salt beds, introducing dissolution waters to promote convective dissolution, pumping out the saturated solution from the pond bottom, and introducing additional dissolution waters.Type: ApplicationFiled: September 24, 2010Publication date: April 14, 2011Inventor: Abraham Sadan
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Patent number: 7815884Abstract: To provide a method for producing polycrystalline silicon at relatively low cost, wherein the amount of waste generated is reduced by decreasing the amount of waste generated in producing polycrystalline silicon from silicon chloride by a method of reduction and increasing the amount of reused auxiliary raw materials. In the production of polycrystalline silicon using a gas phase reaction of a silicon chloride gas and a reducing agent gas, a chlorine gas is blown into an exhaust gas discharged from a reaction device to initiate a reaction, an unreacted reducing agent and silicon particles contained in the exhaust gas are chlorinated, and then a reducing agent chloride contained in the exhaust gas is separated from the other impurities and recovered.Type: GrantFiled: March 19, 2008Date of Patent: October 19, 2010Assignee: Chisso CorporationInventor: Satoshi Hayashida
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Patent number: 7691351Abstract: The present invention is directed to a method for treatment of a gas stream comprising silicon tetrafluoride and hydrogen chloride. For example, the present invention is directed to a method for treatment of such a gas stream that involves contacting the gas stream with a metal that reacts with the hydrogen chloride to provide a treated gas stream having reduced hydrogen chloride content. The present invention is further directed to methods for subjecting silicon tetrafluoride and hydrogen chloride-containing gas streams to elevated pressure to provide gas streams suitable for transport.Type: GrantFiled: September 2, 2008Date of Patent: April 6, 2010Assignee: MEMC Electronic Materials, Inc.Inventors: Vithal Revankar, Jameel Ibrahim
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Patent number: 7371357Abstract: A process for the removal of pollutants from a combustion process and, more particularly, a process for removing pollutants such as carbon dioxide, mercury, sulphur dioxide, nitrogen compounds and oxygen compounds from a combustion process. The process includes the removal of pollutants from a combustion process that produces an emission comprising: cooling the emission to a temperature of about 200° C.; removing nitrogen, water and oxygen from the emission to produce a gas containing a concentration of pollutants; contacting the gas with an aqueous magnesium chloride solution, wherein a slurry mixture is formed; and cooling the gas and the slurry mixture, wherein hydrochloric acid vapour and a sludge are formed.Type: GrantFiled: October 28, 2005Date of Patent: May 13, 2008Assignee: Clean World Strategies Corp.Inventors: Lionel Magumbe, Douglas S. Scott
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Patent number: 6849199Abstract: Snow and ice-melting granules prepared from compacted blends of salts of alkali and/or alkaline earth metals and a method for preparing such granules, are provided. The inventive granules have improved mechanical properties and, as such, are not readily reduced to a powder when subjected to mechanical loadings during transit and storage. In a preferred embodiment, the inventive granules employ one or more corrosion inhibitors homogeneously distributed throughout the granules.Type: GrantFiled: January 21, 2003Date of Patent: February 1, 2005Assignee: Global Specialty Chemicals LLCInventors: Davis R. Vickers, Jr., Thomas P. McGonigle
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Patent number: 6692710Abstract: The present invention provides methods for the isolation and production of magnesium products from leaching of laterite material with acid. A magnesium compound is formed by downstream treatment of a leach stream after at least one of nickel or cobalt have been brought into solution. Magnesite is then obtained by adding at least one of alkali metal or alkaline earth metal carbonate to the leach stream. The magnesite may be converted into magnesium chloride by adding an acid, such as HCL.Type: GrantFiled: March 22, 2001Date of Patent: February 17, 2004Assignee: Crew Development CorporationInventor: Brian J. Ballou
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Patent number: 6524546Abstract: A new process for producing calcium chloride and other metal halides from the carbonates, bicarbonates, oxides of these metals. The process utilizes the discovery that hydrogen halides, when used in a true or conventional fluidizing medium in shallow beds of the aforementioned solids at moderately elevated temperatures in a continuous counter current process results in the conversion of the metal carbonates, bicarbonates, and oxides, into metal halides and carbon dioxide gas and/or water vapor. The process is carried out in a series of true or conventional fluidized beds preferable but not necessarily arranged in a vertical configuration so that the solids flow downward due to the fluidized process and the hydrogen halides flow counter currently in an upward direction producing metal halides at the bottom and pure carbon dioxide gas and/or water vapor at the top.Type: GrantFiled: November 2, 2001Date of Patent: February 25, 2003Inventors: William J. Rigby, Keith D. Cochran, Timothy G. Holt
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Patent number: 6482366Abstract: An apparatus (10) for calcining a material comprises a calcination vessel (10) which houses a heat exchanger (12). The heat exchanger (12) is arranged to transfer heat to the material from a liquid metal heat exchange fluid arranged to flow through the heat exchanger (12).Type: GrantFiled: March 25, 1999Date of Patent: November 19, 2002Assignees: Commonwealth Scientific and Industrial Research Organisation, Australian Magnesium Corporation PTY LTDInventors: Ivars Mirovics, Malcolm Timothy Frost, Raymond Louis Koenig, Peter James Tait
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Patent number: 6423292Abstract: Anhydrous MgCl2 is prepared by a) dissolving magnesite in a starting melt of MgCl2—CeCl3 forming MgCl2+CeOCl+CO2↑, b) and converting the CeOCl back to CeCl3 by chlorination with Cl2 in the presence of a reducing agent such as CO2 or H2 to yield a second melt of MgCl2—CeCl3 having a higher concentration of MgCl2. Steps a) and b) are repeated with the second melt to further increase the concentration of MgCl2. The concentrated MgCl2—CeCl3 melt is then reacted with MgO and Cl2 in the absence of a reducing agent to convert the soluble CeCl3 into insoluble CeO2 precipitate which can be separated to yield pure MgCl2.Type: GrantFiled: June 5, 2000Date of Patent: July 23, 2002Inventor: Ram A. Sharma
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Patent number: 6296790Abstract: A method of producing magnesium chloride granules with a particle size in the range from 0.4 to 3.0 mm suitable for fluidization, air drying and chlorinating to anhydrous state, by preparing a feed solution of MgCl2 having a 30-55% by weight of MgCl2, feeding the solution and keeping it at high temperatures from the feeding tank to the nozzles, atomisation of the feed solution into the bed of already dried particles by pressure or compressed air, passing preheated air upwardly through the bed, maintaining the particles in a fluidizing state and a bed temperature between 100-170° C., continuously recovering entrained particles in a cyclone, discharging magnesium chloride particles continuously, classifying discharged material and recycling of any undersized fraction and crushed oversize fraction together with fines from the cyclone to the fluid bed for further granulation.Type: GrantFiled: April 9, 1999Date of Patent: October 2, 2001Assignee: Norsk Hydro ASAInventors: Birger Langseth, Arne Bent Frigstad, Leif K{dot over (a)}re Grønstad
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Patent number: 6231822Abstract: A method of recovering chloride and sulfate salts from spent potliner using acid digestion.Type: GrantFiled: November 30, 1998Date of Patent: May 15, 2001Assignee: Goldendale Aluminum CompanyInventors: Robert J. Barnett, Michael B. Mezner
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Patent number: 6143270Abstract: Anhydrous magnesium chloride is prepared by a process in which hydrated magnesium chloride (10) is mixed in a vessel (11) with ethylene glycol (12). The mixture (13) is dehydrated in distillation columns (14, 15 and 16) with the dehydrated ethylene glycol magnesium chloride solution (20) pumped into a crystalliser (21) simultaneously with the separate addition of anhydrous ammonia gas (22) to the crystalliser (21). Prior to the introduction of reactants (20 and 22), the crystalliser (21) contains ethylene glycol saturated with ammonia. A crystalliser slurry of magnesium chloride hexammoniate (23) is continuously pumped from the crystalliser (21) into a pressure filter (24) where the crystals are washed with methanol saturated with ammonia (26). The washed crystals (27) are transferred to a fluidised bed calciner (28) where methanol is evaporated from the crystals at 120.degree. C. and thereafter the crystals are calcined to anhydrous magnesium chloride at 450.degree. C.Type: GrantFiled: April 29, 1996Date of Patent: November 7, 2000Assignees: Commonwealth Scientific and Industrial Research Organisation, Australian Magnesium Corporation Pty Ltd.Inventors: Gregory John Sheehan, Fook-Sin Wong, Michael Matthew Hourn, Manabu Kodama, David Hughes Jenkins
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Patent number: 6042794Abstract: A process for producing anhydrous magnesium chloride comprising steps of selective calcination of Mg-containing minerals, selective leaching of magnesium, separation of insoluble impurities, precipitation of magnesium chloride hexammoniate and thermal decomposition of the magnesium chloride hexammoniate crystals into magnesium chloride and ammonia.Type: GrantFiled: January 15, 1999Date of Patent: March 28, 2000Assignee: Norsk Hydro ASAInventors: Ketil Amundsen, Hans Ragnar Eklund, Ralf Schmidt
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Patent number: 5866088Abstract: Disclosed is a process for preparing an anhydrous magnesium halide solution, comprising a step of distilling water off from an oxygen-containing organic solvent solution of hydrous magnesium halide containing at least calcium as an impurity, to prepare an oxygen-containing organic solvent solution of anhydrous magnesium halide, wherein a potassium compound is added in said step to precipitate calcium and potassium, followed by removing the calcium and potassium. According to this process, an anhydrous magnesium halide solution scarcely containing calcium can be prepared from hydrous magnesium halide containing calcium as an impurity. Also disclosed is a process for preparing a solid titanium catalyst component for olefin polymerization, comprising contacting the anhydrous magnesium halide solution obtained by the above process with a liquid titanium compound to precipitate a solid titanium catalyst component.Type: GrantFiled: March 28, 1997Date of Patent: February 2, 1999Assignee: Mitsui Chemicals, Inc.Inventors: Yoshinao Itoh, Masayuki Takeda
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Patent number: 5607655Abstract: A generally dipyramidal-shaped catalyst precursor is prepared by dissolving magnesium dichloride and a suitable alcohol in a suitable solvent and then cooling to obtain a precipitate of the desired shape. The use of the precursor to prepare catalysts and the use of the catalysts to prepare polymers is also disclosed.Type: GrantFiled: March 6, 1995Date of Patent: March 4, 1997Assignee: Phillips Petroleum CompanyInventors: Joel L. Martin, Gil R. Hawley
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Patent number: 5565080Abstract: In accordance with the present invention, there is now provided a process for the production an anhydrous magnesium chloride-containing melt or electrolyte containing very low levels of MgO, typically less than 0.2% by weight MgO, directly from hydrated magnesium chloride feeds. More specifically, the process comprises the steps of a) feeding hydrated magnesium chloride in a furnace containing molten electrolyte from a magnesium electrolysis cell to produce a melt, the temperature in the furnace being maintained between 450.degree. and 65.degree. C.; b) simultaneously injecting an anhydrous hydrogen chloride-containing gas into the melt in an amount below the stoichiometric requirement of 2 moles of HCl per mole of magnesium chloride produced from hydrated magnesium chloride, and agitating the melt to keep any magnesium oxide in suspension in them melt, to dehydrate the magnesium chloride and react with the MgO in the melt so that the melt contains not more than 0.Type: GrantFiled: April 12, 1995Date of Patent: October 15, 1996Assignee: Noranda Metallurgy Inc.Inventors: John G. Peacey, Mark W. Kennedy, Thomas P. Walker
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Patent number: 5556820Abstract: A solid product as a catalyst component for an olefin polymerization catalyst is obtained by the reaction of metallic magnesium, an alcohol, and a halogen in an amount ranging from 0.019 to 0.06 gram-atom per one mole of metallic magnesium. Alternatively, the halogen component is a halogen-containing compound which contains not less than 0.0001 gram-atom of a halogen atom per one gram-atom of metallic magnesium.Type: GrantFiled: March 2, 1994Date of Patent: September 17, 1996Assignee: Idemitsu Petrochemical Co., Ltd.Inventors: Hideo Funabashi, Akinobu Sugahara, Akira Tanaka, Masatoshi Toda, Tsuyoshi Ota, Youichi Matsuo, Tsutomu Akimaru, Sigeo Iwasaki, Masayuki Tsuruoka
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Patent number: 5514359Abstract: In a process for producing anhydrous magnesium chloride, the following combination of steps: drying impure salt containing hydrated magnesium chloride; establishing a solution of the hydrated magnesium chloride; removing insoluble impurities; reacting the solution of hydrated magnesium chloride at substantially ambient temperature and pressure by feeding it into an ammonia saturated very low boiling point alcohol solution and in the presence of ammonium chloride while maintaining the last-mentioned solution saturated in ammonia thereby to form a precipitate of ammoniated magnesium chloride; separating the precipitate and heating it to obtain anhydrous MgCl.sub.2 and ammonia for recycling.Type: GrantFiled: December 20, 1994Date of Patent: May 7, 1996Assignee: Alcan International LimitedInventors: Olivo G. Sivilotti, Jean V. Sang, Rejean J. R. Lemay
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Patent number: 5455018Abstract: Crystalline MgCl.sub.2 particulates, exhibiting the morphology of substantially regular polyhedra having an even number of from 10 to 18 face surfaces, are well suited as support substrate for olefin polymerization catalysts.Type: GrantFiled: May 17, 1993Date of Patent: October 3, 1995Assignee: Elf Atochem S.A.Inventors: Claude Brun, Jean-Michel Brusson, Laurent Duranel, Roger Spitz
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Patent number: 5277889Abstract: Metal halide compositions of enhanced purity are produced by vapor phase deposition via reactions involving organometallic starting materials in a process wherein a carbon getter is provided in the reaction zone and/or adjacent the developing metal halide deposit. The carbon getter reduces carbon contamination in the product which can result from side decomposition reactions involving the organometallic starting materials.Type: GrantFiled: May 13, 1985Date of Patent: January 11, 1994Assignee: Corning IncorporatedInventors: Joseph M. Power, Ahmad Sarhangi
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Patent number: 5212133Abstract: Porous particles of MgCl.sub.2 which have essentially the shape of two truncated right cones connected by their larger bases, which truncated cones are incurved towards the axis of symmetry perpendicular to the bases, at the intersection of the envelope of the truncated cones with two orthogonal planes passing through the said axis of symmetry. These particles are impregnated with a transition metal compound and employed as a catalytic component in the polymerization of olefins. The resultant polyolefins, especially polyethylene, polypropylene and their copolymers, are comprised of particles with a distinctive structure.Type: GrantFiled: February 19, 1991Date of Patent: May 18, 1993Assignee: AtochemInventors: Laurent Duranel, Jean-Pierre Roche
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Patent number: 5212132Abstract: Porous particles of MgCl.sub.2 having the form of essentially regular polyhedrons with six or eight faces in which the paired symmetrically opposite faces are essentially parallel, two of which faces are large and elongated and form the top face and the bottom face of a polyhedron such that on each of them the longest diagonal (D) is larger than the shortest distance (d) separating two opposite sides, which large elongated faces are surrounded essentially perpendicularly by the other essentially rectangular faces that form the sides of the said polyhedron, the length of the smaller side (e) of each of the said essentially rectangular faces being less than the shortest distance (d) separating the two opposite sides of the large elongated faces, catalytic components supported on the particles, catalyst systems utilizing the catalytic products, process for making the particles, and polyolefins obtained utilizing the catalytic systems.Type: GrantFiled: November 22, 1991Date of Patent: May 18, 1993Assignee: AtochemInventors: Roger Spitz, Thierry Soto, Claude Brun, Laurent Duranel
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Patent number: 5112584Abstract: Method for production of magnesium chloride, to be used for production of magnesium, by leaching of magnesite in hydrochloric acid. A two-stage leaching process is used where in a first reactor magnesite lumps are dissolved in hydrochloric acid. The magnesium chloride containing solution is led to a second reactor, where finely ground magnesite or hydrochloric acid is added to obtain approximate equivalence between magnesium and chlorine. To precipitate the impurities an excess of magnesium oxide or magnesium hydroxide is added in one or several purification stages.Type: GrantFiled: April 17, 1990Date of Patent: May 12, 1992Assignee: Norsk Hydro a.s.Inventors: Glor T. Mejdell, Hanne M. Baumann, Kjell W. Tveten
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Patent number: 5089094Abstract: In a process for the electrolytic production of magnesium by the molten salt electrolysis of magnesium chloride using a molten salt cell bath comprised mainly of one or more salts selected from alkali metal chlorides and alkaline earth metal chlorides, the molten salt bath is enriched with magnesium chloride by suspending a magnesium oxide and/or magnesium carbonate powder to form a molten suspension and passing a chlorine-containing gas through the molten suspension at a temperature of 600.degree.-900.degree. C. so as to react the suspended powder with chlorine to form magnesium chloride. The resulting molten salt enriched with magnesium chloride can be directly introduced into the cell for electrolysis, thereby eliminating moisture absorption by the highly hygroscopic magnesium chloride. A pure magnesium can be produced with a high yield and improved current efficiency.Type: GrantFiled: March 15, 1990Date of Patent: February 18, 1992Assignee: Osaka Titanium Company LimitedInventors: Tadashi Ogasawara, Yoshitake Natsume, Kenji Fujita
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Patent number: 5061470Abstract: Improved processes for the production of silane. Hydridomagnesium chloride and trichlorosilane are reacted in an ether solvent to co-produce silane and magnesium chloride. Recycle schemes are presented for the recovery of magnesium values.Type: GrantFiled: August 3, 1990Date of Patent: October 29, 1991Assignee: Ethyl CorporationInventor: Won S. Park
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Patent number: 4981674Abstract: A process for the preparation of anhydrous magnesium chloride containing acceptable amounts of MgO suitable for use in the electrolytic production of magnesium metal comprises the steps of feeding spray-dried magnesium chloride powder, or a magnesite or magnesia powder to a furnace containing a molten magnesium chloride melt at a temperature of about 750.degree.-850.degree. C., and reacting the melt with a carbonaceous reductant and chlorine. The gases are introduced using a gas disperser consisting of a rotating vaned impeller with a tube in the center of the impeller to create gas bubbles having a diameter smaller than 5 nm and having a gas hold-up as high as 30% of the original melt volume, and also ensure that the fine particles present in the melt are evenly suspended.Type: GrantFiled: August 2, 1989Date of Patent: January 1, 1991Assignee: Noranda, Inc.Inventor: John G. Peacey
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Patent number: 4957722Abstract: A process for producing chlorides by the chlorination of a material selected from the group consisting of aluminous materials and metal and metalloid oxides in the presence of a reductant. The method comprises calcining a carbonaceous material with added steam to oxidize substantially all precursors of chlorinated hydrocarbons and to form a reductant; and chlorinating a material selected from the group consisting of aluminous materials and metal oxides in the presence of the reductant.Type: GrantFiled: April 3, 1989Date of Patent: September 18, 1990Assignee: Aluminum Company of AmericaInventors: Raouf O. Loutfy, Kirk R. Weisbrod, James C. Withers
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Patent number: 4943426Abstract: A method for regulating the temperature at which two or more substances combine to form end product in the reactor, at least one of said substances produced from two or more reactants in the reactor, said method comprising: combining at least some of the reactants in a vessel thermally isolated from the reactor to produce substance in the vessel; and transferring substance from said vessel to the reactor. The invention constitutes an improved method for producing magnesium chloride by heating magnesium carbonate in packed bed reactor; passing carbon monoxide and chlorine gas through the packed bed; and withdrawing carbon dioxide from above the packed bed and molten magnesium chloride from below said bed. This improvement consists essentially of reacting at least some carbon monoxide and chlorine in a continuously-cooled vessel to form phosgene; and substituting a sufficient amount of phosgene from the vessel for the carbon monoxide and chlorine gas otherwise passed through said packed bed.Type: GrantFiled: June 20, 1988Date of Patent: July 24, 1990Assignee: Aluminum Company of AmericaInventors: LeRoy E. Dastolfo, Jr., Vito Cedro, III.
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Patent number: 4851208Abstract: A process for the manufacture of substantially spherical particles of at least one metal compound of Group II of the Periodic Table, comprising dissolving such compound in a solvent therefor to form a solution and introducing the solution into a non-solvent medium; said non-solvent medium consisting essentially of at least two liquids that are non-solvents for said compound, at least one of said non-solvents being immiscible with the solvent solution and at least one of said non-solvents being miscible with said solvent solution.Type: GrantFiled: July 21, 1986Date of Patent: July 25, 1989Assignee: AtochemInventors: Laurent Duranel, Nadine Sanchez
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Patent number: 4650778Abstract: Metal halide particles useful, among other things, as olefin polymerization catalyst precursors and catalyst supports are prepared by vaporizing the metal halide and then condensing it in the presence of a diluent.Type: GrantFiled: January 18, 1985Date of Patent: March 17, 1987Assignee: E. I. Du Pont de Nemours and CompanyInventors: Ulrich Klabunde, Rolf Mulhaupt
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Patent number: 4563339Abstract: In electrolytic production of magnesium metal the concentration of magnesium chloride in the bath is required to be replenished periodically or continuously. This magnesium chloride should be anhydrous and of certain specifications.This invention provides a method for the production of such anhydrous magnesium chloride in a two-stage dehydration of magnesium chloride solution, the first step consisting of preparation of a fine powder from magnesium chloride with 0.5 to 1.5 molecules of water and about 4 to 10% magnesium oxide with or without alkali or alkaline earth metal chlorides, or both depending on the starting material. This first step is carried out in a conventional apparatus like the spray drier, briquetting the above partially dehydrated product in admixture with carbon powder under pressure to obtain compacted material such as briquettes of bulk density of 0.6 to 1.3 g/c.c., and size 1.5 to 5 cm. Second step comprises heating the above briquettes to a temperature of 200.degree. to 350.degree. C.Type: GrantFiled: March 6, 1984Date of Patent: January 7, 1986Assignee: Council of Scientific and Industrial ResearchInventors: Panchapagesa Subramanian, Arunachalam Selvakesavan, Laguduva K. I. Srinivasan, Poonamalle Srinivasadesikan, Kadathur S. Srinivasan, Gajavalli N. R. Kannan, Somasundaram Sukumaran, Narasimhan Rajagopalan, Koyalmannam S. Dhandapani, Chanassery O. Augustin, Thangaraj S. Devasahayam, Srinivasa Srikantan, Handady V. Udupa
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Patent number: 4532313Abstract: Disclosed is a transition metal component of a Ziegler-Natta catalyst which is composed of a titanium halide deposited on an essentially anhydrous magnesium chloride support. An improved support is prepared by contacting a hydrocarbon solution of magnesium alkanoate and a hydrocarbon solution of alkylaluminum dichloride in a liquid hydrocarbon reaction medium containing alkylaluminum dichloride and alkylaluminum alkanoate chloride. After workup and treatment with the titanium halide, the transition metal component is used in the Ziegler-Natta catalysis polymerization of 1-olefins. The resulting polyolefins have a narrow particle size distribution and a high bulk density.Type: GrantFiled: August 20, 1984Date of Patent: July 30, 1985Assignee: HIMONT IncorporatedInventor: Albert S. Matlack
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Patent number: 4474703Abstract: An organometallic halide having the formula:(RMX) (MX.sub.2).sub.a (MR.sub.2).sub.b (MH.sub.2).sub.cwherein a.ltoreq.0.45, b.ltoreq.0.15, and c.ltoreq.0.30, X is a halogen, R is a hydrocarbon radical, and M is a metal selected from the group consisting of magnesium, zinc, beryllium, and calcium is prepared by a continuous dry process by reacting an organic monohalide RX and a metal M in the form of convex solid grains of a size between 1 and 15 mm. The reaction temperature is lower than the temperature at which decomposition of the organometallic halide RMX begins and at least 10.degree. C. higher than the boiling point of the organic monohalide. The reaction may also take place in the presence of an organometallic derivative comprising a hydroxy group or an enolysable ketone group. The resulting organometallic halide may be used for the synthesis of anhydrous magnesium halide or for the reduction of titanium tetrachloride.Type: GrantFiled: September 22, 1982Date of Patent: October 2, 1984Assignee: Societe Chimique des Charbonnages-CdF ChimieInventors: Karel Bujadoux, Jean-Marie Neyer, Jean-Pierre Houzeaux
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Patent number: 4401641Abstract: A new crystalline form (beta form) of MgCl.sub.2 is disclosed, as are methods for obtaining it by reaction of SOCl.sub.2 with hydrated MgCl.sub.2 at a temperature comprised between room temperature and the boiling point of SOCl.sub.2.Type: GrantFiled: December 28, 1981Date of Patent: August 30, 1983Assignee: Montedison S.p.A.Inventors: Enrico Albizzati, Ivano Bassi, Giorgio Foschini, Sandro Parodi, Franco Pirinoli
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Patent number: 4382019Abstract: This invention relates to pretreating the support material for a polymerization catalyst comprising magnesium chloride with an active hydrogen compound such as an organic acid phosphate or a phenol in order to transform substantially elemental magnesium and other impurities. The impure magnesium chloride originates as a by-product from the manufacture of magnesium alkyls by the reaction of alkyl chlorides with elemental magnesium. Succeeding steps are activating the support material with an electron donor and treating the activated product with a titanium halide.The invention also includes the novel catalytic component containing titanium halide, itself, the process for making that component, use of this catalytic system for polymerizing olefins such as propylene, and the purification step for magnesium chloride, itself.Type: GrantFiled: September 10, 1981Date of Patent: May 3, 1983Assignee: Stauffer Chemical CompanyInventor: Carl C. Greco
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Patent number: 4366140Abstract: An organometallic halide having the formula:(RMX)(MX.sub.2).sub.a (MR.sub.2).sub.b (MH.sub.2).sub.cwherein a.congruent.0.45, b.congruent.0.15, and c.congruent.0.30, X is a halogen, R is a hydrocarbon radical, and M is a metal selected from the group consisting of magnesium, zinc, beryllium, and calcium is prepared by a continuous dry process by reacting an organic monohalide RX and a metal M in the form of convex solid grains of a size between 1 and 15 mm. The reaction temperature is lower than the temperature at which decomposition of the organometallic halide RMX begins and at least 10.degree. C. higher than the boiling point of the organic monohalide. The reaction may also take place in the presence of an organometallic derivative comprising a hydroxy group or an enolysable ketone group. The resulting organometallic halide may be used for the synthesis of anhydrous magnesium halide or for the reduction of titanium tetrachloride.Type: GrantFiled: March 30, 1981Date of Patent: December 28, 1982Assignee: Societe Chimique des Charbonnages-CdF ChimieInventors: Karel Bujadoux, Jean-Marie Neyer, Jean-Pierre Houzeaux
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Patent number: 4302433Abstract: Substantially anhydrous magnesium chloride is prepared through the chlorination of a hydrated magnesium chloride by melting the hydrated chloride, feeding that molten material to a bed of carbonaceous material so that it flows downwardly therethrough and simultaneously feeding a mixture of chlorine and air to the bed of carbonaceous material so that it flows upwardly therethrough countercurrent to the molten material, until magnesium chloride of the desired state of purity is obtained, and the purified magnesium chloride is then recovered.Type: GrantFiled: May 2, 1977Date of Patent: November 24, 1981Assignee: Anic S.p.A.Inventor: Richard B. Stein
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Patent number: 4269816Abstract: The invention relates to a process for the preparation of anhydrous magnesium chloride from magnesium carbonate preferably magnesium carbonate ores such as magnesite. The process comprises reacting solid magnesium carbonate pieces preferably screened ore in a packed bed reactor comprising the magnesium carbonate pieces with gaseous chlorine in the presence of carbon monoxide at a temperature above the melting point of magnesium chloride and below 1200.degree. C. The off-gas predominantly carbon dioxide is withdrawn from above the packed bed and molten anhydrous magnesium chloride is withdrawn from below the packed bed. The invention provides a process having low energy requirements which can be applied industrially on a continuous basis using simple apparatus.Type: GrantFiled: July 27, 1979Date of Patent: May 26, 1981Assignee: Mineral Process Licensing Corp. BVInventors: Charles E. E. Shackleton, deceased, by Edward A. B. Shackleton, executor, Anthony J. Wickens, John H. W. Turner
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Patent number: 4248838Abstract: This invention outlines a process to beneficiate carnallite ores in such a way as to obtain anhydrous MgCl.sub.2 of sufficient purity to be used as feed for an electrolysis cell producing magnesium metal. Commercially acceptable potassium chloride as also recovered. The organic solvents and the anhydrous ammonia used to obtain the beneficiation of these carnallite materials are recovered for recycle in the process.Type: GrantFiled: March 21, 1979Date of Patent: February 3, 1981Assignee: Nalco Chemical CompanyInventors: Ronald J. Allain, David G. Braithwaite, Joseph P. Maniscalco
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Patent number: 4248839Abstract: Magnesium oxide is chlorinated in molten impure magnesium chlorine with chlorine gas by adding ferrous chloride to magnesium chloride brine, drying the brine, adding a mixture of calcined petroleum coke and charcoal to the dried brine, melting the product and chlorinating the formed melt. Ferrous chloride is added in amounts sufficient to provide from about 1.0% to 2.2% by weight of iron in the dried product. A highly reactive carbon source is added in amounts of from about 0.8 to 2.3% by weight and a carbon source that is less reactive than the highly reactive carbon source is added in amounts ranging from about 0.8 to 2.3% by weight of dried brine. Iron levels in the magnesium chloride melt may be adjusted upwardly by addition of a mixture of iron oxide and charcoal.A melt cell characterized by side entry electrodes disposed at angles from 40.degree. to 50.degree., an arched roof configuration, and an improved electrode refractory and ceramic sleeve construction is used to chlorinate the magnesium.Type: GrantFiled: July 30, 1979Date of Patent: February 3, 1981Assignee: NL Industries, Inc.Inventors: Robert D. Toomey, Brian R. Davis, Ramaswami Neelameggham, R. Keith Darlington
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Patent number: 4228144Abstract: Anhydrous magnesium chloride containing substantially no magnesium oxide is produced by a process comprising reacting magnesium chloride in the form of its hexahydrate with ammonia in the presence of ammonium chloride in an aqueous media; separating the resultant precipitated magnesium chloride hexammoniate crystals from an aqueous solution containing unreacted ammonia, magnesium chloride and ammonium chloride; washing the crystals with liquid ammonia; decomposing the washed crystals into anhydrous magnesium chloride and gaseous ammonia, and; isolating the anhydrous component from the composition mixture; which process is characterized in that a portion of the separated aqueous solution is evaporated until the concentration of ammonia in the resulting residual liquid becomes 2.Type: GrantFiled: February 16, 1979Date of Patent: October 14, 1980Assignee: Ube Industries Ltd.Inventors: Hisashi Kono, Kenji Terai, Takazumi Niwa, Katsumi Uemura, Tetsuya Oda
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Patent number: 4201758Abstract: A method for removing boric acid and salts therefrom from ethylene glycol-magnesium chloride solutions which contain at least 100 ppm of boron which comprises reducing the pH of such solutions below 7 and then adding thereto at least 3 moles of methanol based on the amount of boric acid or salt thereof present in said solution and then subjecting the thus-treated ethylene glycol-magnesium chloride solution to distillation at a temperature sufficient to remove trimethyl borate-methanol therefrom, thereby reducing the level of boron in the starting solution to not more than 35 ppm.Type: GrantFiled: March 22, 1979Date of Patent: May 6, 1980Assignee: Nalco Chemical Co.Inventors: Ronald J. Allain, David G. Braithwaite, Ansell L. Reid
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Patent number: 4195071Abstract: In a process of producing anhydrous magnesium chloride of the type comprising:A. Mixing together a magnesium chloride hydrate, said hydrate containing minor amounts of water-soluble sulfate and boron compounds as impurities with diethyl ether of tetraethylene glycol to prepare 0.1-6.0% by weight slurry of MgCl.sub.2 in the diethyl ether of tetraethylene glycol and an azeotropic agent having a boiling point less than the diethyl ether of tetraethylene glycol in a quantity sufficient to remove water from said slurry;the improvement which comprises substituting dibutyl ether of tetraethylene glycol for the diethyl ether of tetraethylene glycol.Type: GrantFiled: March 1, 1979Date of Patent: March 25, 1980Assignee: Nalco Chemical CompanyInventors: Ronald J. Allain, David G. Braithwaite, Joseph P. Maniscalco
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Patent number: 4195070Abstract: A method of beneficiating a mixed salt mineral ore containing potassium and magnesium sulfates and/or their hydrates which allows the recovery of anhydrous magnesium chloride and the simultaneous recovery of commercially acceptable potassium sulfate.Type: GrantFiled: March 21, 1979Date of Patent: March 25, 1980Assignee: Nalco Chemical CompanyInventors: Ronald J. Allain, David G. Braithwaite, Joseph P. Maniscalco