Utilizing Acid Patents (Class 423/626)
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Patent number: 4166100Abstract: The method of preparing granulated activated alumina consists in that alumina trihydrate is decomposed by bringing it in contact with a bed of a solid heat carrier having the temperature of 350.degree. to 600.degree. C., the contact time being from 0.05 to 0.5 second, to obtain a product of decomposition in the form of amorphous aluminium hydroxide. Said decomposition product is mixed with water into a suspension having the concentration of 100-500 g/liter, calculating with reference to aluminium oxide, and hydrated at a temperature of 20.degree.-100.degree. C. and the pH of 5 to 12 for 0.5 to 10 hours. The hydrated decomposition product is then treated with an acid, that can form water-soluble basic salts of aluminium, at a temperature of 20.degree. to 150.degree. C., granulated, dried at a temperature of 20.degree. to 150.degree. C., and calcined at a temperature of 400.degree. to 600.degree. C.Type: GrantFiled: May 26, 1978Date of Patent: August 28, 1979Inventors: Jury K. Vorobiev, Boris N. Badaev, Galina I. Ljubushko, Emmanuil A. Levitsky, Georgy K. Boreskov, Mikhail M. Andrushkevich, Bronislav A. Baum, Nikolai A. Pakhomov, Ljudmila G. Khomyakova, Alexandr E. Khramov, Nina A. Rodionova, Boris N. Isaev, Vladimir M. Knyazev, Ella M. Moroz, Vladimir N. Erofeev, Ivan P. Druzhinin, Rimma A. Shkrabina
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Patent number: 4159313Abstract: Alumina agglomerates with high mechanical strength and selectable particle size are obtained by compacting an intermediate product resulting from incomplete decomposition of a substance of the group comprising hexahydrated aluminum chloride, hydrated aluminum nitrate, hydrated aluminum sulfate of the formula Al.sub.2 O.sub.3, xSO.sub.3, yH.sub.2 O and hydrated aluminum sulfite of the formula Al.sub.2 O.sub.3, xSO.sub.2, yH.sub.2 O, which after thermal decomposition contain from 0.5 to 15% by weight of Cl, of nitrogen oxide expressed as N.sub.2 O.sub.5 or of sulfur expressed as SO.sub.3 or SO.sub.2, which compacted product is then granulated and the granulated product subjected to heat treatment.Type: GrantFiled: July 22, 1977Date of Patent: June 26, 1979Assignee: Aluminum PechineyInventors: Henry Mercier, Joseph Cohen, Pierre Maurel
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Patent number: 4154812Abstract: An alumina composition comprising a microcrystalline boehmite-pseudoboehmite intermediate having from about 70 to about 85 weight percent of the total amount of Al.sub.2 O.sub.3 present in crystalline form. The composition is prepared by adding aluminum sulfate and sodium aluminate solutions to a mixture of water and aluminum sulfate solution to precipitate alumina and adjusting the pH to a pH higher than the precipitation pH. The reactant concentrations, and rates of addition, temperatures, and pH's in the precipitation are specifically controlled to form the boehmite-pseudoboehmite intermediate.Type: GrantFiled: March 25, 1977Date of Patent: May 15, 1979Assignee: W. R. Grace & Co.Inventors: Moises G. Sanchez, Norman R. Laine
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Patent number: 4151267Abstract: Pure alumina is produced from aluminum metal by steps of activation by stripping the oxide layer in an acidic aqueous medium; washing in a neutral medium; reacting in a neutral, acidic or alkaline medium to give hydrated alumina; and igniting the hydrated alumina.Type: GrantFiled: August 8, 1977Date of Patent: April 24, 1979Inventor: Ferenc Puskas
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Patent number: 4120942Abstract: Disclosed is a method for forming shaped catalysts from a rehydratable alumina composition. The method includes a staged rehydration procedure to stabilize the rehydratable alumina to facilitate extrusion processing.Type: GrantFiled: October 17, 1978Date of Patent: October 17, 1978Assignee: American Cyanamid CompanyInventors: Donald P. Spitzer, William Edward Bambrick
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Patent number: 4116882Abstract: Alumina spheres are formed by peptizing alumina slurries, centrifugates, and filtercakes, aging and dropping the peptized material through a hydrocarbon filled column. The improved method avoids the drying and reslurrying of alumina powders currently used and provides a method whereby harmful ions such as chloride and sulfates can be excluded from the alumina.Type: GrantFiled: December 14, 1977Date of Patent: September 26, 1978Assignee: Continental Oil CompanyInventors: Larry L. Bendig, Cathy S. Siemsen, Donald E. Stowell
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Patent number: 4102978Abstract: Alumina catalyst carriers are produced by bonding pre-fired gibbsite with microcrystalline boehmite. Superior strength of the product is achieved by use of gibbsite fired to an L.O.I. at 1000.degree. C of 8% or less, or preferably less than 4%.Type: GrantFiled: May 20, 1977Date of Patent: July 25, 1978Assignee: Norton CompanyInventor: Joseph R. Kiovsky
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Patent number: 4102821Abstract: A method for preparing a hydrotreating catalyst having a controlled pore distribution is disclosed. The method requires adding to the alumina prior to forming from 0.1 to 15% by weight of a water soluble polycarboxylic acid having from 2 - 22 carbon atoms. The resulting formed alumina support after being calcined has a pore volume distribution such that most of the pore volume in pores greater than 200 A in diameter as measured by Mercury penetration porosimitry is substantially eliminated. The pore volume as measured by nitrogen adsorption in the range of between 100 A and 1200 A is reduced. The polycarboxylic acid may be added to the catalyst carrier prior to forming in different ways such as by dissolving the catalytically active metals with the water soluble polycarboxylic acid and then impregnating hydrothermally or by pore volume or by adding a water soluble polycarboxylic acid salt to the hydrous or xero gel after precipitation.Type: GrantFiled: May 31, 1977Date of Patent: July 25, 1978Assignee: Nalco Chemical CompanyInventor: George N. Pessimisis
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Patent number: 4093707Abstract: A peroxide group containing complex of aluminum, oxygen and hydrogen is obtained having an aluminum/oxygen atomic ratio of about 1:3.The complex is prepared by reacting, at a temperature below 150.degree. F, aluminum metal of a purity of at least 99.98% by weight with a source of hydrogen ions, such as an aqueous inorganic halogen acid, in the presence of mercury and an oxygen gas-containing atmosphere, the aluminum being partially immersed in the mercury and the source of hydrogen ions, comprising a thin film over the mercury. The thickness of this film is insufficient to cover the aluminum not immersed in the mercury, whereby a portion of the aluminum is exposed to the oxygen gas-containing atmosphere. The complex grows from the exposed surface of the aluminum in the form of an easily frangible self-supporting sheet.Type: GrantFiled: November 17, 1975Date of Patent: June 6, 1978Inventor: George G. Merkl
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Patent number: 4048295Abstract: Formed products are made from aqueous aluminum oxyhydrate by peptizing the aqueous aluminum oxyhydrate with an acid and then subsequently adding a dilute solution of ammonia or an ammonia yielding compound following by extrusion, drying and calcining.Type: GrantFiled: December 16, 1975Date of Patent: September 13, 1977Assignee: Condea Chemie GmbHInventors: Martin Wassermann, Arnold Meyer
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Patent number: 4045234Abstract: Sintered alumina of low porosity and Na content is made from calcined alumina of 2-6 micron average particle size and about 0.2-1% by weight Na.sub.2 O content by treating the calcined alumina with a synergistically acting combination of a magnesium salt and a boron compound. Suitable magnesium salts include magnesium halides, nitrate, sulfate, acetate and stearate, the water-soluble salts being preferred. As boron compound H.sub.3 BO.sub.3 or B.sub.2 O.sub.3 can be employed. The quantity of magnesium salt in the combination, calculated as Mg, is kept in the range of about 0.01-0.3% by weight of Al.sub.2 O.sub.3, while the boron content, calculated as B.sub.2 O.sub.3, is maintained in the range of about 0.1-1% by weight of Al.sub.2 O.sub.3. Used of the synergistically acting combination in the indicated range allows manufacture of sintered alumina products of less than about 3% total porosity and less than about 0.03% by weight Na content.Type: GrantFiled: August 23, 1976Date of Patent: August 30, 1977Assignee: Kaiser Aluminum & Chemical CorporationInventor: Terry A. Ring
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Patent number: 4034067Abstract: The preparation of a material consisting essentially or largely of aluminum hydroxychlorides having the general formula Al.sub.2 (OH).sub.X Cl.sub.6.sub.-X, in which X is a value up to 5 or more and obtained by reacting active alumina, secured by partial dehydration of hydrates of alumina, with hydrochloric acid or aluminum chloride in which the active alumina has a specific surface area of at least 200 m.sup.2 /g.Type: GrantFiled: May 17, 1976Date of Patent: July 5, 1977Assignee: Rhone-Poulenc IndustriesInventors: Laurent Seigneurin, Michel Brunet
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Patent number: 4032623Abstract: A hydroperoxy-group-containing aluminum compound is prepared by a process which comprises:Contacting and reacting, at room temperature or below, and in the substantial absence of water, (a) a reactive metal comprising aluminum of a purity of at least 99.9% by weight permeated with a liquid metal selected from mercury, gallium and indium/gallium alloys with (b) a liquid reactant comprising (i) hydrogen peroxide in (ii) a liquid organic compound having no multiple carbon-to-carbon bonds.The aluminum compounds produced can be used, for example, as substrates for electronics, in the preparation of synthetic gems, ceramics and paint pigments. The aluminum compound is prepared in sheet for plate form, resembling mica in physical appearance.In an alternative embodiment, a metal or metal salt is added to the reactive system to yield a hydroperoxy-group-containing aluminum compound with the desired metal deposited thereon.Type: GrantFiled: August 16, 1976Date of Patent: June 28, 1977Inventor: George G. Merkl
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Patent number: 4032472Abstract: A sufficient amount of alumina is initially digested in aqueous hydrochloric or hydrofluoric acid to provide from about 5 to about 25 wt. % of the aluminum content of the desired alumina sol, and a finely divided aluminum is subsequently digested therein to provide the remaining required amount of alumina. The method enables the digestion reaction to be effected at an increased rate, and affords a sol of improved homogeniety and reproducibility.Type: GrantFiled: January 7, 1976Date of Patent: June 28, 1977Assignee: UOP Inc.Inventor: Kenneth R. McCallister
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Patent number: 4028216Abstract: A stoichiometric amount of aluminum is commingled with hydrochloric acid in an aqueous media to provide a final reaction mixture containing from about 10 to about 14 wt. % aluminum in from about a 1:1 to about 1.5:1 ratio with the chloride anion content thereof. The mixture is treated in the presence of a soluble salt of cobalt or nickel at conditions effecting substantially complete digestion of the aluminum.Type: GrantFiled: May 30, 1975Date of Patent: June 7, 1977Assignee: Universal Oil Products CompanyInventor: Edward Michalko
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Patent number: 4010247Abstract: Water dispersible aluminum hydroxide is prepared by treating an acid dispersible aluminum hydroxide with 1 to 9 weight % of a gaseous acid.Type: GrantFiled: February 10, 1975Date of Patent: March 1, 1977Assignee: CONDEA Petrochemie-Gesellschaft m.b.H.Inventors: Martin Wilhelm Wassermann, Arnold Wilhelm Meyer
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Patent number: 4003737Abstract: Method of agglomerating solids in a liquid suspension utilizing in the bridging liquid an additive chemically active with respect to such solids. The solid to be agglomerated is suspended in a first liquid which is, or is made to be, at least relatively nonwetting with respect thereto. A second immiscible or bridging liquid is then introduced into said first liquid. Said second liquid is, or contains dissolved therein material which is, reactive to such solid material. The entire system is then agitated and the solid material thereby formed into agglomerates. The use of a chemically reactive material in the bridging liquid provides a wide range of selectability of and control over the properties, either physical or chemical, of the resulting agglomerates.Type: GrantFiled: July 22, 1974Date of Patent: January 18, 1977Assignee: Canadian Patents and Development LimitedInventors: Bruce F. Caswell, I. E. Puddington
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Patent number: 3997476Abstract: High pore volume alumina materials which are particularly effective catalyst supports are prepared by treating a calcined alumina with an organic acid such as ethanedioic acid. The acid treatment changes the pore structure of the alumina and particularly increases the macroporosity of the alumina.Type: GrantFiled: July 8, 1975Date of Patent: December 14, 1976Assignee: Exxon Research and Engineering CompanyInventor: Neville L. Cull
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Patent number: 3983212Abstract: A method of producing an alumina bearing product in which the alumina is substantially soluble in cold alkali including the steps of contacting an aluminium bearing material with concentrated sulphuric acid containing 30 to 100 weight percent sulphuric acid, heat treating the acid and material to cause the acid to react with the material to form a substantially anhydrous hard product and decomposing the product by heat treatment to produce the alumina bearing product. The alumina values may be recovered from the resulting alumina bearing product using the known Bayer process. The process has particular application to non-bauxitic ores.Type: GrantFiled: August 29, 1974Date of Patent: September 28, 1976Inventors: Hyman Moses Lowenstein, Arthur Michael Lowenstein
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Patent number: 3975510Abstract: Low-density, high-porosity alumina extrudates and a method for preparing said extrudates. Said method comprises admixing finely divided low-density, high-porosity alumina with water to form an extrudable composition and extruding said mixture.Type: GrantFiled: April 14, 1975Date of Patent: August 17, 1976Assignee: Continental Oil CompanyInventors: Bruce E. Leach, George G. Hritz, Dennis Jack Royer
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Patent number: 3975509Abstract: Alpha alumina monohydrate wherein a majority of the cumulative pore volume consists of pores from about 30 to about 120 A in diameter and a method for producing such alumina. This is a continuation of application Ser. No. 298,116, filed Oct. 16, 1972 and now abandoned.Type: GrantFiled: April 3, 1975Date of Patent: August 17, 1976Assignee: Continental Oil CompanyInventors: Dennis Jack Royer, George G. Hritz
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Patent number: 3969273Abstract: A process for the preparation of phosphate-containing extruded alumina catalyst supports is disclosed. Due to their particular characteristics, these supports find application in hydrocarbon conversion catalysts and especially in catalysts for the hydrotreating of petroleum feedstocks.Type: GrantFiled: April 24, 1975Date of Patent: July 13, 1976Assignee: W. R. Grace & Co.Inventors: Stanley Monty Brown, David Nelson Wallace
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Patent number: 3968225Abstract: A process for preparing aluminium oxide beads from alumina hydrogel, which comprises polymerizing, in a hot and substantially water-immiscible fluid, an aqueous mixture comprising alumina hydrogel and alumina hydrosol and a water-soluble monomer whose uncross-linked polymer is water-soluble or forms a gel, this mixture being dispersed as droplets into a hot fluid in which substantial polymerization of the monomer occurs.Type: GrantFiled: February 10, 1975Date of Patent: July 6, 1976Assignee: Labofina S.A.Inventors: Jacques Maurice Jules Ghislain Andre, Raymond Mark Cahen, Henri Robert Debus, Rene Odon Lammers, Hugo Johannes VAN Thillo
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Patent number: 3966996Abstract: A process for preparing aluminum oxide beads from alumina hydrogel, comprising polymerizing in a hot and substantially water-immiscible fluid, an aqueous mixture which contains alumina hydrogel and a water soluble monomer whose uncross-linked polymer is water soluble or forms a gel, this mixture being dispersed as droplets into said fluid in which substantial polymerization of said monomer is performed.Type: GrantFiled: February 10, 1975Date of Patent: June 29, 1976Assignee: Labofina S.A.Inventors: Jacques Maurice Jules Andre, Hugo Johannes VAN Thillo, Rene Odon Lammers, Henri Robert Debus, Raymond Marc Cahen
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Patent number: 3954957Abstract: Alumina monohydrate crystals of uniform particle size in the range of 0.2-0.7 microns suitable for use as pigments in paper, paints, or ink are produced by grinding Bayer trihydrate to a median particle size of 1-3 microns followed by digestion in the presence of a controlled amount of mineral acid.Type: GrantFiled: February 24, 1975Date of Patent: May 4, 1976Assignee: Aluminum Company of AmericaInventor: James J. Koenig
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Patent number: 3950507Abstract: The invention relates to a method for producing granulated porous corundum having a homogeneous porous structure with a total pore volume of 0.3 to 1.0 cm.sup.3 /g and predominant pore size of 5000 to 30000 A. The method comprises subjecting the granules of active alumina or aluminum hydroxide having a porous structure with a total pore volume of 0.3 to 1.0 cm.sup.3 /g and pore size of 20 to 5000 A to heat treatment by increasing the temperature from 20.degree.C to 700.degree.C during a period of at least 0.5 hour, thereafter the granules are heat treated at a temperature range of from 700.degree.C to 1000.degree.C for at least 0.5 hour, and then at a temperature range of from 1000.degree.C to 1400.degree.C for at least 0.5 hour, the heat treatment in the temperature range of from 20.degree.C to 1000.degree.C being carried out in an atmosphere of hydrogen fluoride which is present in amounts of from 0.01 to 2.0 percent of the weight of active alumina.Type: GrantFiled: March 19, 1974Date of Patent: April 13, 1976Inventors: Georgy Konstantinovich Boreskov, Valentina Nikclaevna Kuklina, Emmanuil Aronovich Levitsky, Boris Nikolaevich Badaev, Vladimir Alexandrovich Balashov
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Patent number: 3945945Abstract: High surface area alumina bodies for use as catalysts, catalyst carriers, and sorbents are made by controlled mixing of fine particle size platy boehmite alumina aggregates with a monobasic acid to produce non-pasty free-flowing particulate mass of aggregates of boehmite. This mass can then be formed by pressure into selected shapes such as rings, saddles, cylinders, solid, or hollow, or pellets, dried and fired to produce bodies of boehmite, gamma alumina, delta alumina, theta alumina or alpha alumina ranging in surface area of from 10 square meters per gram to greater than 300 square meters per gram. Catalytic metal can be included in the bodies by impregnation, before or after firing, or can be incorporated by inclusion in the aqueous acid treating solution.Type: GrantFiled: January 16, 1973Date of Patent: March 23, 1976Assignee: Norton CompanyInventors: Joseph R. Kiovsky, Jeffrey W. Meacham
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Patent number: 3944658Abstract: A transparent, activated, nonparticulate alumina with a total porosity of about 63% which consists of a unique pore morphology and size distribution and is thermally stable up to about 1,200.degree.C. at which temperature it can be nondestructively converted to alpha alumina is disclosed as well as a method of preparing said alumina by hydrolyzing aluminum alkoxides to form a particular sol which is essentially clear to the naked eye and the gel of which retains its integrity during drying and pyrolysis. The alumina thus produced is useful as a catalyst, absorbent and desiccant. In addition, a method of preparing the intermediate clear colloidal sol or gel consisting essentially of aluminum monohydrate is disclosed. This intermediate can be used to coat various substrates.Type: GrantFiled: September 13, 1973Date of Patent: March 16, 1976Assignee: Owens-Illinois, Inc.Inventor: Bulent E. Yoldas
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Patent number: 3941719Abstract: A transparent, activated, nonparticulate alumina with a total porosity of about 63% which consists of a unique pore morphology and size distribution and is thermally stable up to about 1200.degree.C. at which temperature it can be nondestructively converted to alpha alumina is disclosed as well as a method of preparing said alumina by hydrolyzing aluminum alkoxides to form a particular sol which is essentially clear to the naked eye and the gel of which retains its integrity during drying and pyrolysis. The alumina thus produced is useful as a catalyst, absorbent and desiccant. In addition, a method of preparing the intermediate clear colloidal sol or gel consisting essentially of aluminum monohydrate is disclosed. This intermediate can be used to coat various substrates.Type: GrantFiled: September 10, 1973Date of Patent: March 2, 1976Assignee: Owens-Illinois, Inc.Inventor: Bulent E. Yoldas