By Precipitating Or Gelling From Silicate Solution Patents (Class 423/333)
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Patent number: 5776893Abstract: A crystalline hydrated layered sodium and potassium silicate/amorphous sodium and potassium silicate composite material with predetermined hardness ion sequestration properties is achieved by controlling the process for forming the material. The process for producing the crystalline hydrated layered sodium and potassium silicate/amorphous is sodium and potassium silicate composite comprises hydrolyzing DB-1 crystalline sodium and potassium silicate glasses as a precursor material to produce the composite material known as DB-2. Hydrolysis of the DB-1 precursor material is achieved by adding typically up to 100.0 milliequivalents per gram of H.sub.3 O.sup.+ ions or up to 50 milliequivalents per gram of OH.sup.- ions. The resulting DB-2 material can sequester CA.sup.2+ ions, Mg.sup.+ ions, or both, depending on the results desired, processing conditions, and starting materials used.Type: GrantFiled: June 6, 1995Date of Patent: July 7, 1998Assignee: PQ CorporationInventors: Eric Von Rehren Borgstedt, Raymond P. Denkewicz, Jr.
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Patent number: 5772979Abstract: Process for manufacturing an alkali metal aluminosilicate of zeolite wherein zeolite P seeds are produced in situ in a first reacting gel with a SiO.sub.2 /Al.sub.2 O.sub.3 ratio of above 2.2 and it is only after the formation of zeolite P seeds, but before said seeds have the time to fully grow, that sodium aluminate is added in order to get a gel which can have a SiO.sub.2 /Al.sub.2 O.sub.3 ratio of about 2 which therefore enables producing a zeolite P having also a SiO.sub.2 /Al.sub.2 O.sub.3 ratio of about 2.Type: GrantFiled: December 19, 1996Date of Patent: June 30, 1998Assignee: Crossfield LimitedInventor: Abraham Araya
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Patent number: 5739098Abstract: A crystalline silicate material containing both sodium and potassium cations within the crystalline matrix. Wherein the material is SiO.sub.2 /(xNa.sub.2 O+yK.sub.2 O)=Z where x+y=1, 0.75<x<1.0 (and therefore 0.0<y<0.25), and 1.3.ltoreq.Z.ltoreq.3.22. The material possesses predetermined superior hardness ion sequestration properties determined by the composition and processing of the material. The material can be made by any one of several processes which are also set forth.Type: GrantFiled: July 5, 1994Date of Patent: April 14, 1998Assignee: PQ CorporationInventors: Raymond P. Denkewicz, Jr., Eric von Rehren Borgstedt
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Patent number: 5707598Abstract: A porous material composed of many SiO.sub.4 tetrahedra sheets having interlayer bridges of SiO.sub.2. It has pores having a diameter of 10 .ANG. or above, and possesses the properties of a solid acid formed by the isomorphous substitution of metal atoms for Si of SiO.sub.4 frameworks. It is made by a process including introducing an organic substance into interlayer space of crystals of layered silicates to expand the spacing between crystal layers, as well as forming bridges of SiO.sub.2 therebetween, bringing the intercalated compounds into contact with a metal salt to link metal atoms to the SiO.sub.4 frameworks, and firing the products. The material can withstand a temperature of 800.degree. C., has a pore diameter larger than that of zeolites, etc., and is useful in making an adsorbent or catalyst for molecules having a high molecular weight, such as a catalyst for the catalytic cracking of petroleum.Type: GrantFiled: February 7, 1994Date of Patent: January 13, 1998Assignee: Kabushiki Kaisha Toyota Chuo KenkyushoInventors: Shinji Inagaki, Yoshiaki Fukushima, Akane Okada, Chuzo Kato, Kazuyuki Kuroda
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Patent number: 5693304Abstract: A particulate amorphous alkali metal silicate is prepared by heating a mixture of silicate glass and water or aqueous solution to a temperature of about 300.degree.-400.degree. C. to provide a foamed material that is easily formed into particles of less than 20 microns. After careful hydration, a product having 1-15% water based on loss of ignition (LOI) of product at 800.degree. C. is produced that controls the activity of magnesium in solutions and is, therefore, a useful detergent ingredient.Type: GrantFiled: June 1, 1995Date of Patent: December 2, 1997Assignee: PQ CorporationInventors: Eric von Rehren Borgstedt, Raymond P. Denkewicz, Jr.
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Patent number: 5643358Abstract: The present invention pertains to a crystalline hydrated layered sodium and potassium silicate/amorphous sodium and potassium silicate composite material with predetermined hardness ion sequestration properties achieved by controlling the process for forming the material. The process for producing the crystalline hydrated layered sodium and potassium silicate/amorphous sodium and potassium silicate composite comprises hydrolyzing DB-1 crystalline sodium and potassium silicate glasses as a precursor material to produce the composite material known as DB-2. Hydrolysis of the DB-1 precursor material is achieved by adding typically up to 100.0 milliequivalents per gram of H.sub.3 O.sup.+ ions or up to 50 milliequivalents per gram of OH.sup.- ions. The resulting DB-2 material can sequester CA.sup.2+ ions, Mg.sup.+ ions, or both, depending on the results desired, processing conditions, and starting materials used.Type: GrantFiled: November 3, 1994Date of Patent: July 1, 1997Assignee: PQ CorporationInventors: Eric von Rehren Borgstedt, Raymond P. Denkewicz, Jr.
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Patent number: 5614161Abstract: The invention relates to a crystalline sheet sodium silicate of the general formulaxNa.sub.2 O.multidot.ySiO.sub.2 .multidot.zP.sub.2 O.sub.5in whichthe ratio of x to y corresponds to a number from 0.35 to 0.6,the ratio of x to z corresponds to a number from 1.75 to 1200and the ratio of y to z corresponds to a number from 4 to 2800,a process for its preparation and its use.Type: GrantFiled: February 21, 1996Date of Patent: March 25, 1997Assignee: Hoechst AktiengesellschaftInventors: Jan Wilkens, Gunther Schimmel
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Patent number: 5614160Abstract: The present invention pertains to a crystalline hydrated layered sodium silicate/amorphous sodium silicate composite material with predetermined hardness ion sequestration properties achieved by control of the process for forming the material, and a process for making the material. The process for producing the crystalline hydrated layered sodium silicate/amorphous sodium silicate composite consists of producing a crystalline sodium disilicate by heating a sodium silicate at a specified time and temperature. The resulting material may include amorphous material, and the crystalline sodium disilicate can be either alpha-phase or delta-phase disilicate. This crystalline sodium disilicate is then hydrolyzed with up to 50.0 milliequivalents per gram of either H.sub.3 O.sup.+ ions or OH.sup.- ions. The resulting material can sequester Ca.sup.2+ ions, Mg.sup.2+ ions, or both, depending on the results desired, processing conditions, and starting materials used.Type: GrantFiled: June 10, 1994Date of Patent: March 25, 1997Assignee: PQ CorporationInventors: Petra M. Gill, Eric von Rehren Borgstedt, Raymond P. Denkewicz, Jr.
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Patent number: 5595716Abstract: A novel synthetic mixed-layer silicate consisting of the layers of serpentine and layers of saponite each having a specified chemical composition is proposed, which has excellent dispersibility in water to form a colloidal dispersion capable of being converted into a gel by standing to be useful as a gelating agent exhibiting thixotropy along with unique porosity characteristics which enable the use thereof as an adsorbent.Type: GrantFiled: August 18, 1995Date of Patent: January 21, 1997Assignee: Japan as directed by Director General of Agency of Industrial Science and TechnologyInventors: Kazuo Torii, Takashi Iwasaki, Yoshio Onodera
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Patent number: 5567404Abstract: An improved layered sodium silicate having a .delta. crystalline structure and a process for preparing it is described. By pulverizing anhydrous sodium silicate into an anhydrous sodium silicate powder, adding a limited mount of water to form a mixture granulating the mixture, and directly calcining the granules, a layered sodium silicate having improved calcium ion binding capacity and magnesium ion binding capacity can be produced.Type: GrantFiled: September 1, 1994Date of Patent: October 22, 1996Assignee: Korea Research Institute of Chemical TechnologyInventors: Jung-Min Lee, Jeong-Kwon Suh, Soon-Yong Jeong, Chun-Hee Park, Jeong-Hwan Park
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Patent number: 5547603Abstract: The invention concerns a solid alkalimetal silicate having a molar ratio SiO.sub.2 :M.sub.2 O from about 1.5 to about 3, in which M is an alkali metal and substantially consists of sodium and optionally potassium. The silicate contains from about 7 to about 20% by weight of sodium carbonate based on the dry material and has a water content from about 14 to about 22% by weight. Further, the invention concerns a method of preparing the silicate above, use of the same and cleaning agent compositions containing such a silicate.Type: GrantFiled: May 13, 1994Date of Patent: August 20, 1996Assignee: Eka Nobel ABInventors: Olle Sorensson, Krister Severinsson
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Patent number: 5503820Abstract: An improved method for preparing low-concentration polysilicate microgels from a water soluble silicate and a strong acid in which the silicate and acid are mixed at a rate to produce a Reynolds number of at least 4000, the mixture is aged and then diluted to a silica concentration of not more than 1.0 wt. %. The method achieves reduced silica deposition during the preparation of the microgels.Type: GrantFiled: November 28, 1994Date of Patent: April 2, 1996Assignee: E. I. Du Pont de Nemours and CompanyInventors: Robert H. Moffett, John D. Rushmere
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Patent number: 5503819Abstract: Novel fluoride containing substituted smectite clays are disclosed as well as their preparation and uses. The clay has the formulaA.sub.x (M.sub.y M'.sub.4--y)(Si.sub.8--x M.sub.t M'.sub.v)O.sub.20 (OH).sub.4--u F.sub.uwhere A is a cation, M and M' are metals having a +3 oxidation state, each selected from the group consisting of aluminum, gallium, iron and chromium, x is the moles of A, y is the moles of M, t and v are the moles of M and M' in the tetrahedral layer and t+v=x and u is the moles of F. The clay composition may be used as is or after pillaring to catalyze hydrocarbon conversion processes such as alkylation.Type: GrantFiled: March 18, 1994Date of Patent: April 2, 1996Assignee: UOPInventor: Jennifer S. Holmgren
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Patent number: 5456895Abstract: The present invention relates to a process for the production of crystalline sodium sheet silicate with kanemite structure with the chemical formulaNaH Si.sub.2 O.sub.5 .multidot.X H.sub.2 Oin which X represents a value between 1 and 3. Crystalline sodium sheet silicate with kanemite structure is produced by maintaining a mixture of sodium disilicate, silica and water in the molar ratio of 1:2:(6-8) at a temperature of 20.degree. to 100.degree. C. for a period of 0.2 to 10 h.Type: GrantFiled: May 18, 1994Date of Patent: October 10, 1995Assignee: Hoechst AktiengesellschaftInventors: Alexander Tapper, Renate Adrian, Gunther Schimmel
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Patent number: 5435988Abstract: The invention relates to a process for the preparation of crystalline clathrasil of the dodecasil 1 H structural type having an average crystal size of not more than 20 .mu.m, characterised in that an alkaline aqueous silicate-containing medium comprising templates and crystallisation seeds is heat-treated, the crystallisation seeds content, relative to the SiO.sub.2 content of the medium, being not less than 1% by weight.Type: GrantFiled: March 2, 1993Date of Patent: July 25, 1995Assignee: Merck Patent Gesellschaft mit Beschrankter HaftungInventors: Michael Grebner, Axel Reich, Ferdi Schuth, Klaus Unger
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Patent number: 5427758Abstract: The invention relates to a process for the preparation of mixtures of synthetic, crystalline magadiite and salts which split off oxygen. For this purpose, 1 mol of soda-water glass which has a molar ratio of SiO.sub.2 :Na.sub.2 O=1:(0.25 to 0.5) is mixed with 0.1 to 0.9 mol of a compound which has a pH of less than 10.5 in molar aqueous concentration, as a neutralizing agent. In the presence of magadiite seed crystals, the reaction mixture is heated at temperatures from 373 to 523 K. in an autoclave for 1 to 15 hours and, after cooling, 0.15 to 1.5 mol of hydrogen peroxide are added per mol of soda-water glass employed. The solid and the dissolved substances are isolated from the reaction suspension as dry substance.Type: GrantFiled: February 28, 1994Date of Patent: June 27, 1995Assignee: Hoechst AktiengesellschaftInventor: Harald Bauer
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Patent number: 5424053Abstract: The invention relates to a process for the preparation of mixtures of synthetic, crystalline kenyaite and salts which split off oxygen. For this purpose, 1 mol of soda-water glass which has a molar ratio of SiO.sub.2 :Na.sub.2 O=1:(0.25 to 0.5) is mixed with 0.1 to 0.9 mol of a compound which has a pH of less than 10.5 in molar aqueous concentration, as a neutralizing agent. In the presence of kenyaite seed crystals, the reaction mixture is heated at temperatures from 373 to 523 K. in an autoclave for 1 to 10 hours and, after cooling, 0.15 to 1.5 mol of hydrogen peroxide are added per mol of soda-water glass employed. The solid is isolated from the reaction suspension as dry substance.Type: GrantFiled: February 28, 1994Date of Patent: June 13, 1995Assignee: Hoechst AktiengellschaftInventor: Harald Bauer
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Patent number: 5417951Abstract: The invention is a process for the hydrothermal production of crystalline sodium disilicate by heating an aqueous mixture of quartz sand and sodium hydroxide or an aqueous solution of sodium disilicate with a solids content of at least 50% by weight or more than 75% by weight at a temperature above 235.degree. C. and under autogenous pressure to form crystalline sodium disilicate.Type: GrantFiled: June 1, 1993Date of Patent: May 23, 1995Assignee: Henkel Kommanditgesellschaft auf AktienInventor: Guenther Just
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Patent number: 5365002Abstract: The invention relates to a crystalline zeolite-like gallosilicate having an atomic ratio of Si/Ga in the outer crystalline surface that is not larger than the average Si/Ga ratio for the whole of the crystal. The invention also relates to a method of making such a gallosilicate comprising the hydrothermal crystallization of a strictly inorganic reaction mixture having the following molar ratios: SiO.sub.2 /Ga.sub.2 O.sub.3 .gtoreq.5; OH.sup.- /SiO.sub.2 =0.05-1.0; and H.sub.2 O/SiO.sub.2 =10-1,000. The invention further relates to the above-described method wherein said reaction mixture is prepared by adding an aged gel to a first mixture, the first mixture preferably having a composition with the following molar ratios: SiO.sub.2 /Ga.sub.2 O.sub.3 .gtoreq.5; OH.sup.- /SiO.sub.2 =0.05 to 1.0; and H.sub.2 O/SiO.sub.2 =20 to 100.Type: GrantFiled: June 24, 1992Date of Patent: November 15, 1994Assignees: VAW Aluminium AG, Veba OEL AGInventors: Martin Wallau, Rudolf Spichtinger, Klaus K. Unger, Arno Tissler, Roland Thome
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Patent number: 5362466Abstract: The invention describes a process for preparing P zeolites in which aluminate and silicate solutions are reacted in the presence of a P-zeolite seed.Type: GrantFiled: April 8, 1993Date of Patent: November 8, 1994Assignee: Unilever Patent Holdings B.V.Inventor: Abraham Araya
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Patent number: 5354548Abstract: This invention provides a three dimensional inorganic oxide structure comprising a myriad of cavities interconnected by holes having a narrow pore size distribution, in which the diameters of the cavities is in the range from 1 to 50 .mu.m and that of the holes in the range 1 to 10 .mu.m and in which the pore volume in the range 1 to 10 .mu.m is at least 2 cc/g and in which the inorganic oxide is selected from alumina, silica, titania, zirconia and mixtures thereof and a process for the preparation of such structures.Type: GrantFiled: November 2, 1992Date of Patent: October 11, 1994Assignee: Unilever Patent Holdings B.V.Inventors: Abraham Araya, Anthony L. Lovell
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Patent number: 5344633Abstract: The invention concerns a solid alkalimetal silicate having a molar ratio SiO.sub.2 :M.sub.2 O from about 1.5 to about 3, in which M is an alkalimetal substantially consisting of sodium and potassium. The silicate contains from about 1 and up to about 5% by weight of K.sub.2 O based on the dry material and the water content being from about 16 to about 25% by weight based on the total weight.Further, the invention concerns a method of its preparation, its use and a cleaning agent composition containing the silicate above.Type: GrantFiled: June 14, 1993Date of Patent: September 6, 1994Assignee: Eka Nobel ABInventors: Olle Sorensson, Krister Severinsson
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Patent number: 5338528Abstract: The invention concerns a solid alkalimetal silicate having a molar ratio SiO.sub.2 :M.sub.2 O from about 1.5 to about 3, in which M is an alkalimetal and substantially consists of sodium and optionally potassium. The silicate contains from about 7 to about 20% by weight of sodium carbonate based on the dry material and has a water content from about 14 to about 22% by weight.Further, the invention concerns a method of preparing the silicate above, use of the same and cleaning agent compositions containing such a silicate.Type: GrantFiled: June 14, 1993Date of Patent: August 16, 1994Assignee: Eka Nobel ABInventors: Olle Sorensson, Krister Severinsson
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Patent number: 5308596Abstract: To prepare crystalline sodium disilicates having a laminar structure, a molar ratio of SiO.sub.2 to Na.sub.2 O of (1.9 to 2.1) 1 and a water content of less than 0.3% by weight, a water glass solution is first obtained by reacting sand with sodium hydroxide solution in a molar ratio of SiO.sub.2 to Na.sub.2 O of (2.0 to 2.3) : 1 at temperatures of 180.degree. to 240.degree. C. and pressures of 10 to 30 bar. This water glass solution having at least 20% by weight of solids is treated in a spray drier with hot air at 200.degree. to 300.degree. C. with the formation of a pulverulent amorphous sodium disilicate having a water content (determined as loss on heating at 700.degree. C.) of 15 to 23% by weight and a bulk density of at least 300 g/l. The spray-dried pulverulent, amorphous sodium disilicate is ground.Type: GrantFiled: December 8, 1992Date of Patent: May 3, 1994Assignee: Hoechst AktiengesellschaftInventors: Michael Kotzian, Gunther Schimmel, Alexander Tapper, Knut Bauer
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Patent number: 5268156Abstract: To prepare crystalline sodium silicates having a laminated structure, a molar ratio of SiO.sub.2 to Na.sub.2 O of (1.9 to 2.1) 1 and a water content of less than 0.3% by weight from a water glass solution which has a solids content of at least 20% by weight and is obtained by reaction of sand with sodium hydroxide solution in a molar ratio of SiO.sub.2 : Na.sub.2 O of (2.0 to 2.3) : 1, the water glass solution is treated with hot air of 200.degree. to 300.degree. C. in a spray drying zone to form a pulverulent, amorphous sodium silicate having a water content (determined as the loss on ignition at 700.degree. C.) of 15 to 23% by weight. The pulverulent, amorphous, water-containing sodium silicate is first ground, preferably to particle sizes of 1 to 50 .mu.m, before it is introduced into an inclined rotary tubular oven and treated in this in countercurrent with flue gas at temperatures of more than 500.degree. to 850.degree. C. to form crystalline sodium silicate.Type: GrantFiled: February 21, 1992Date of Patent: December 7, 1993Assignee: Hoechst AktiengesellschaftInventors: Gunther Schimmel, Michael Kotzian, Alexander Tapper, Gerd Wingefeld
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Patent number: 5238668Abstract: A process is disclosed for the hydrothermal production of potassium silicate solutions with high SiO.sub.2 :K.sub.2 O molar ratios, by the hydrothermal reaction of quartz sand with aqueous potassium hydroxide solutions at temperatures in the range of 150.degree. to 300.degree. C. at the pressures of saturated water vapor corresponding to these temperatures in a pressure reactor, which is characterized in that the potassium silicate solutions obtained thereby, which have SiO.sub.2 :K.sub.2 O molar ratios of less than 2.75:1, are then reacted with a quartz tempered at temperatures in the range of over 1100.degree. C. up to melting point, the temperatures and pressures also being maintained in the ranges named.Type: GrantFiled: May 26, 1992Date of Patent: August 24, 1993Assignee: Henkel Kommanditgesellschaft auf AktienInventors: Rudolf Novotny, Alfred Hoff, Jost Schuertz
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Patent number: 5236681Abstract: There is provided a method for synthesizing layered silicates such as magadiite and kenyaite. The source of silica used in this method is freshly precipitated from a silicate solution. For example, this silica source may be obtained by treating an aqueous solution of sodium silicate with sulfuric acid to form an amorphous silica precipitate. This silica precipitate is not dried to reduce its activity prior to use.Type: GrantFiled: November 30, 1989Date of Patent: August 17, 1993Assignee: Mobil Oil Corp.Inventors: Pochen Chu, Garry W. Kirker, Sowmithri Krishnamurthy, James C. Vartuli
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Patent number: 5219813Abstract: There is described a process for the preparation of novel crystalline molecular sieves, characterized by a distinctive x-ray diffraction pattern and a chemical composition in terms of mole ratios of oxides in the anhydrous state by the formula aX.sub.2 O:bM.sub.2 O.sub.3 :cSiO.sub.2 where X is a mixture of monovalent cation selected from the group consisting of alkali metal, ammonium and hydrogen, M is selected from Al, B, Fe, Ga, Cr or mixtures thereof and a=0.0 to 1.0, b=0.0 to 1.0 and c=20 or above.Type: GrantFiled: January 3, 1992Date of Patent: June 15, 1993Assignee: Council of Scientific & Industrial ResearchInventors: Rajiv Kumar, Korandla R. Reddy, Paul Ratnasamy
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Patent number: 5211930Abstract: For the preparation of crystalline sodium silicates having a sheet structure and an SiO.sub.2 /Na.sub.2 O molar ratio of 1.9:1 to 3.5:1 from waterglass solutions having a solids content of 20 to 65% by weight, the waterglass solutions are first treated in a spray-drying zone. This gives a pulverulent amorphous sodium silicate having a maximum ignition loss of 20% by weight, while the waste gas leaving the spray-drying zone is at a temperature of at least 140.degree. C. Thereafter, the spray-dried sodium silicate is heated in an ignition zone containing an agitated solid bed at temperatures of 500.degree. to 800.degree. C. for 1 to 60 minutes in the presence of at least 10% by weight of recycled material. This recycled material was obtained by mechanical comminution of crystalline sodium silicate discharged from the ignition zone.Type: GrantFiled: April 26, 1991Date of Patent: May 18, 1993Assignee: Hoechst AktiengesellschaftInventors: Gunther Schimmel, Reinhard Gradl, Martin Schott
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Patent number: 5187132Abstract: A method for synthesizing crystalline zeolites requiring a reaction mixture for crystallization thereof which contains Boron Beta Zeolite as an active source of silicon oxide and boron oxide.Type: GrantFiled: May 14, 1991Date of Patent: February 16, 1993Assignee: Chevron Research and Technology CompanyInventors: Stacey I. Zones, Lun T. Yuen, Susan D. Toto
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Patent number: 5160718Abstract: A kenyaite-type phyllosilicate having a crystallographically single phase is produced by hydrothermally reacting a mixture containing amorphous silica, a sodium compound, a potassium compound and water at a tempeature of 100.degree.-180.degree. C. wherein the mixture has a composition providing the following molar ratios:H.sub.2 O/SiO.sub.2 : 15-20,sodium compound/SiO.sub.2 : 0.18-0.30potassium compound/SiO.sub.2 : 0.005-0.30sodium compound/potassium compound: 1.1-25.Type: GrantFiled: March 13, 1991Date of Patent: November 3, 1992Assignee: Director-General of Agency of Industrial Science and TechnologyInventors: Katsunori Kosuge, Atsumu Tsunashima
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Patent number: 5130110Abstract: Process for obtaining by sol-gel route refractory metal oxides based on silica in which a monolithic gel is prepared, in an aqueous medium, at a temperature of less than 60.degree. C., by leaving at rest an aqueous sol obtained by simple mixing in stoichiometric quantities of an aqueous sol of silicic acid and of one or more aqueous solutions of a water-soluble salt of one or more other constitutive metals of these oxides, then the monolithic gel obtained is calcined at a temperature of less than 1000.degree. C. after it has been dried at a temperature of less than 150.degree. C.Type: GrantFiled: December 18, 1990Date of Patent: July 14, 1992Assignee: Societe Francaise HoechstInventors: Patrice Rouet, Florence Syoen
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Patent number: 5084262Abstract: The direct hydrothermal production of high purity potassium silicate solutions having a high SiO.sub.2 : K.sub.2 O molar ratio by reaction of a silicon dioxide source with aqueous potassium hydroxide solutions is made possible by using a silicon dioxide source that contains a sufficient fraction of cristobalite phase, or by conditioning other crystalline forms of silicon dioxide by heating at or above 1100.degree. C., but below the melting point of silica, before the hydrothermal treatment. Preferably the potassium hydroxide solution has a concentration range of 10 to 40% by weight, and the reaction is carried out in a closed pressure reactor at temperatures of 150.degree. to 300.degree. C. and under saturated steam pressures corresponding to those temperatures.Type: GrantFiled: January 31, 1990Date of Patent: January 28, 1992Assignee: Henkel Kommanditgesellschaft auf AktienInventors: Rudolf Novotny, Alfred Hoff, Jost Schuertz
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Patent number: 5068216Abstract: There is provided a method for pillaring a layered silicate, such as kenyaite, with polymeric oxide by using a single step treatment with a mixture of swelling agent and pillar precursor. The swelling agent may be an organic cation, such as a cetyltrimethylammonium cation, and the pillar precursor may be a compound which is capable of hydrolyzing to form a polymeric oxide. Tetraethylorthosilicate is an example of such a pillar precursor.Type: GrantFiled: April 17, 1991Date of Patent: November 26, 1991Assignee: Mobil Oil CorporationInventors: Ivy D. Johnson, Kenneth G. Simmons
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Patent number: 5023065Abstract: The present invention concerns synthetic mica powder containing from 75 to 99% of the stoichiometrical composition of fluorine and/or having a shape in which the end face of particle is laminated, process for producing such synthetic mica powder, as well as cosmetics having synthetic mica powder blended therewith, in which the synthetic mica powder shows no leaching of fluorine ions and/or improved hold of oils due to lamination at the surface of powder. Accordingly, in this invention, cosmetics excellent in extensibility, gloss, adherence and modability, having appearance of high chroma and of high stability and safety can be obtained.Type: GrantFiled: September 26, 1988Date of Patent: June 11, 1991Assignees: Shiseido Co., Ltd., Topy Kogyo K.K.Inventors: Kazuhisa Ohno, Tetsushi Kosugi, Kenichiro Sugimori, Akitsugu Ando, Masaru Yamamoto, Fukuji Suzuki, Masahiro Nakamura, Nobuhisa Tsujita
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Patent number: 5000933Abstract: The direct hydrothermal production of high purity sodium silicate solutions having a high SiO.sub.2 : Na.sub.2 O molar ratio by reaction of a silicon dioxide source with aqueous sodium hydroxide solutions, or with aqueous sodium silicate solutions having a lower SiO.sub.2 : Na.sub.2 O molar ratio, is made possible by using a silicon dioxide source that contains a sufficient fraction of cristobalite phase, or by conditioning other crystalline forms of silicon dioxide by heating at or above 1100.degree. C., but below the melting point of silica, before the hydrothermal treatment. Preferably the sodium hydroxide solution has a concentration range of 10 to 50% by weight, and the reaction is carried out in a closed pressure reactor at temperatures of 150.degree. to 300.degree. C. and under saturated steam pressures corresponding to those temperatures.Type: GrantFiled: January 31, 1990Date of Patent: March 19, 1991Assignee: Henkel Kommanditgesellschaft auf AktienInventors: Rudolf Novotny, Alfred Hoff, Jost Schuertz
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Patent number: 4987106Abstract: A process for producing a clay mineral of chain structure such as sepiolite and attapulgite. The process comprises suspending a metal silicate gel in an aqueous solution which has a pH value of 3-11 at room temperature and contains a clay mineral of chain structure suspending therein, and then heating the resulting suspension at a temperature below 350.degree. C. According to this process, it is possible to produce a clay mineral of chain structure in a simple, stable manner.Type: GrantFiled: December 27, 1989Date of Patent: January 22, 1991Assignee: Kabushiki Kaisha Toyota Chuo KenkyushoInventors: Tadashi Mizutani, Yoshiaki Fukushima, Haruo Doi, Osami Kamigaito
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Patent number: 4950310Abstract: X-ray crystalline sodium silicates having a sheet structure and an SiO.sub.2 :Na.sub.2 O molar ratio of 1.9 to 3.5 are prepared by dissolving an X-ray crystalline sodium silicate having a sheet structure and an SiO.sub.2 /Na.sub.2 O molar ratio of 1.9:1 to 3.5:1 in water and evaporating the solution at temperatures of 20.degree. to 445.degree. C.For the preparation of detergents or cleaners, a mixture of surfactants and builders, which may also contain fillers, bleaching agents, bleach activators and enzymes, is made into a paste with water, mixed with an X-ray crystalline sheet sodium silicate having an SiO.sub.2 /Na.sub.2 O molar ratio of 1.9:1 to 3.5:1, mixed thoroughly and then spray-dried.Type: GrantFiled: December 8, 1988Date of Patent: August 21, 1990Assignee: Hoechst AktiengesellschaftInventors: Hans-Peter Rieck, Martin Schott, Willy Ott, Werner Gohla
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Patent number: 4942026Abstract: Sodipotassic copper tube silicate species of the family Na.sub.2--2x K.sub.2x CuSi.sub.4 O.sub.10 are synthesized by combining, with an organo silicate at essentially room temperature, stoichiometric amounts of a copper salt, and at least one salt of potassium and sodium, in an aqueous alcohol solution to form a gel. The gel is then sintered at elevated temperature and for a time sufficient to form a crystalline specie of Na.sub.2--2x K.sub.2x CuSi.sub.4 O.sub.10.Type: GrantFiled: May 10, 1989Date of Patent: July 17, 1990Assignee: Hoechst Celanese CorporationInventors: Balaram Gupta, Cheng K. Saw, Malcolm E. Kenny, Bruce A. Harrington
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Patent number: 4933101Abstract: Disclosed are liquid automatic dishwashing detergent compositions containing an insoluble inorganic zinc salt useful for inhibition of glassware corrosion in the dishwasher. These compositions are particularly desirable because use of them in the dishwasher does not result in precipitation of insolubles on the dishware or dishwasher parts.Type: GrantFiled: February 13, 1989Date of Patent: June 12, 1990Assignee: The Procter & Gamble CompanyInventors: William A. Cilley, Rodney M. Wise
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Patent number: 4806327Abstract: A process for the preparation of a crystalline sheet-type alkali metal silicate is described, in which an aqueous solution of an alkali metal silicate or a suspension of an amorphous alkali metal silica having a molar ratio M.sub.2 O (unneutralized)/SiO.sub.2, where M represents an alkali metal, of 0.05:1 to 0.8:1 is allowed to react at temperatures of 70.degree. to 250.degree. C. until the sheet-type alkali metal silicate crystallizes out. After the beginning of crystallization, an acidic compound is added in an amount such that an M.sub.2 O (unneutralized)/SiO.sub.2 ratio of 0.05:1 to 0.8:1 is constantly maintained in the mother liquor of a filtered sample. However, at least an amount corresponding to 5 milliequivalents of H.sup.+ per mole of SiO.sub.2 in the alkali metal silicate used is added. The use of seed crystals of the desired sheet silicate is advantageous.Type: GrantFiled: June 11, 1986Date of Patent: February 21, 1989Assignee: Hoechst AktiengesellschaftInventors: Hans-Peter Rieck, Martin Schott
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Patent number: 4775495Abstract: The process of the present invention comprises adding an alkaline earth metal hydroxide such as barium hydroxide to a radioactive liquid waste containing sodium sulfate as the main component to convert the latter into an insoluble alkaline earth metal salt such as barium sulfate, adding silicic acid to by-product sodium hydroxide to prepare water glass and solidifying the radioactive insoluble alkaline earth metal salt with the water glass. According to this process, exudation of radioactive substances from the solid can be prevented and the solid having a high durability can be obtained at a low cost.Type: GrantFiled: February 6, 1986Date of Patent: October 4, 1988Assignee: Hitachi, Ltd.Inventors: Tatsuo Izumida, Tsutomu Baba, Akihiko Noie, Masaru Sonobe, Makoto Kikuchi
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Patent number: 4770866Abstract: A process for the hydrothermal production of clear sodium silicate solutions by reacting sand and aqueous NaOH solution wherein an excess of 5 to 10% by weight of sand is used and the reaction is conducted in a rotating pressure vessel until 90 to 95% complete, after which it is transferred and completes in a blow-off vessel.Type: GrantFiled: June 6, 1985Date of Patent: September 13, 1988Assignee: Henkel Kommanditgesellschaft auf AktienInventors: Peter Christophliemk, Rudolf Novotny, Juergen von Laufenberg
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Patent number: 4728439Abstract: A method is disclosed for flocculating suspensions containing (a) layered oxide materials intercalated with a hydrophobic swelling agent and (b) nonintercalated hydrophobic swelling agent. The suspension is contacted with a ketone, water, and a cationic organic polymer; the resulting mixture is maintained at a sufficiently alkaline pH to prevent removal of the intercalated swelling agent during the flocculation treatment. This method is particularly useful for preparing swelled layered chalcogenide materials for the introduction of interspathic polymeric chalcogenide precursors in order to form a thermally stable product.Type: GrantFiled: April 30, 1987Date of Patent: March 1, 1988Assignee: Mobil Oil CorporationInventors: Garry W. Kirker, Sowmithri Krishnamurthy
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Patent number: 4657750Abstract: Crystalline silicates and processes for the production thereof are described. These crystalline silicates are of new crystalline structure, which, as determined after calcination in the air at 550.degree. C., have a composition represented by the general formula (I): pM.sub.2/n O.Al.sub.2 O.sub.3.qSiO.sub.2 (the symbols are as defined in the appended claims) and give a X-ray diffraction pattern as shown in Table 2. They are superior in heat resistance and acid resistance, and can be used as catalysts for the conversion of various organic compounds, absorbents, or as catalysts for various reactions. They are produced by reacting an aqueous mixture comprising (a) a silica source, (b) an alumina source, (c) an alkali metal and/or alkaline earth metal source, and (d) ethylene glycol or (e) monoethanolamine at a temperature of 100.degree. to 300.degree. C. till the desired crystalline silicates are formed.Type: GrantFiled: March 18, 1985Date of Patent: April 14, 1987Assignee: Research Association for Petroleum Alternatives DevelopmentInventors: Kozo Takatsu, Noboru Kawata
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Patent number: 4636373Abstract: This invention relates to a new and improved form of crystalline silicate identified as zeolite ZSM-12, to a new and useful improvement in synthesizing said crystalline silicate and to use of said crystalline silicate prepared in accordance herewith as a catalyst for organic compound, e.g. hydrocarbon compound, conversion.Type: GrantFiled: August 30, 1985Date of Patent: January 13, 1987Assignee: Mobil Oil CorporationInventor: Mae K. Rubin
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Patent number: 4632815Abstract: A method is provided for synthesizing a crystalline layered silicate from a specified reaction mixture having a particular composition including a specified organic directing agent, said layered silicate having a structure related to Silica-X.Type: GrantFiled: December 18, 1984Date of Patent: December 30, 1986Assignee: Mobil Oil CorporationInventor: Ernest W. Valyocsik
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Patent number: 4626421Abstract: A method for preparing magadiite is described wherein the reaction mixture for crystallization thereof contains as a promoter, a hydrocarbon substituted urea or amide. The magadiite prepared according to this method may act as a source of silica in preparing crystalline zeolites or molecular sieves.Type: GrantFiled: June 28, 1985Date of Patent: December 2, 1986Assignee: Chevron Research CompanyInventor: Stacey I. Zones
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Patent number: 4619820Abstract: An improved method of synthesizing highly siliceous ZSM-23 zeolitic material is disclosed and claimed. The method comprises preparing a reaction mixture which comprises sources of an alkali metal, an oxide of aluminum (Al.sub.2 O.sub.3), an oxide of silicon (SiO.sub.2), water and a nitrogen-containing organic cation R.sup.+, and having the following composition, in terms of mole ratios:______________________________________ Broad Preferred ______________________________________ SiO.sub.2 /Al.sub.2 O.sub.3 5,000 to .infin. 10,000 to .infin. H.sub.2 O/SiO.sub.2 5 to 200 20 to 100 OH.sup.- /SiO.sub.2 0 to 0.60 0.10 to 0.40 M.sup.+ /SiO.sub.2 0.01 to 2.0 0.10 to 1.0 R.sup.+ /SiO.sub.2 0.01 to 2.0 0.05 to 1.0 ______________________________________wherein M.sup.+ is a cation of an alkali or alkaline earth metal and R.sup.+ is an organic cation of the formula (CH.sub.3).sub.3 N.sup.+ --R.sub.1 --N.sup.+ (CH.sub.3).sub.3 wherein R.sub.Type: GrantFiled: December 13, 1985Date of Patent: October 28, 1986Assignee: Mobil Oil CorporationInventor: Ernest W. Valyocsik
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Patent number: 4585642Abstract: A process for the preparation of crystalline sodium silicates with a molar ratio SiO.sub.2 /Na.sub.2 O of 1.9:1 to 3.5:1 from amorphous sodium silicate is described. To water-containing amorphous sodium silicate with a molar ratio SiO.sub.2 /Na.sub.2 O of 1.7:1 to 3.75:1 and a water content of 5 to 95% by weight is added 0.01 to 30 parts by weight of the crystalline sodium silicate to be prepared (per 100 parts by weight of Na.sub.2 O+SiO.sub.2 in the water-containing amorphous sodium silicate).The reaction mixture is dehydrated by heating. The dehydrated reaction mixture is kept at a temperature of at least 450.degree. C., but below the melting point, until the sodium silicate has crystallized.Type: GrantFiled: May 9, 1985Date of Patent: April 29, 1986Assignee: Hoechst AktiengesellschaftInventor: Hans-Peter Rieck