Alkali Metal Containing (li, Na, K, Rb, Or Cs) Patents (Class 423/332)
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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: 4657879Abstract: The spray-drying of a feed liquid mixture containing dissolved feed elements is used to produce precursor powders of Na.sup.+ -super conducting sodium gadolinium silicate (Na.sub.5 GdSi.sub.4 O.sub.12), (NGS), and sodium yttrium silicate (Na.sub.5 YSi.sub.4 O.sub.12), NYS. Using these powders, very dense (>97% theoretical) solids are obtained on sintering. The resistivities of the NGS and NYS polycrystalline ceramics are 5 and 7 (.OMEGA. cm) respectively at 300.degree. C. and are dependent on the f(NGS) or f(NYS) values. In the case of NYS, the resistivity/f(NYS) relationship takes the form ##EQU1## indicative of resistive and conductive phases mixed more in parallel than in series.Type: GrantFiled: September 25, 1984Date of Patent: April 14, 1987Assignee: Canadian Patents and Developments LimitedInventors: Patrick S. Nicholson, Kimihiro Yamashita
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Patent number: 4642226Abstract: This invention relates to a new and improved form of crystalline silicate having the structure of zeolite Beta, 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: March 29, 1985Date of Patent: February 10, 1987Assignee: Mobil Oil CorporationInventors: Robert B. Calvert, Clarence D. Chang, Mae K. Rubin, Ernest W. Valyocsik
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Patent number: 4640829Abstract: This invention relates to a new and improved form of crystalline silicate having the structure of zeolite ZSM-50, 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: February 3, 1987Assignee: Mobil Oil CorporationInventor: Mae K. Rubin
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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: 4622214Abstract: Crystalline molecular sieve materials such as high silica zeolites are manufactured using an organic template comprising an optically active enantiomer such as an enantiomer of 3(.+-.) methyl piperidine -N,N-dimethyl bromide.A new zeolite materials is identified.Type: GrantFiled: November 8, 1985Date of Patent: November 11, 1986Assignee: Laporte Industries LimitedInventors: Alan E. Comyns, Gareth W. Morris, John P. Sankey
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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: 4591491Abstract: In a process for the conversion of meta-kaolin into an aqueous alkaline suspension of low-grit, water-containing zeolitic sodium aluminosilicate of the smallest particle size having the molar composition:0.9 to 1.1 Na.sub.2 O: 1 Al.sub.2 O.sub.3 : 1.8 to 2.3 SiO.sub.2with a water content depending on the degree of drying, which contains at least 99.8% by weight of a particle size of less than 25.mu. and has a high cation exchange capability, the improvement consisting of:slowly heating a suspension of reactants to a zeolitization temperature in the range of from 70.degree. to 100.degree. C., with a temperature rise averaging 20.degree. C.Type: GrantFiled: July 11, 1984Date of Patent: May 27, 1986Assignee: Henkel Kommanditgesellschaft auf AktienInventors: Peter Christophliemk, Willi Wust
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Patent number: 4589988Abstract: Softener-containing washing agents which, in addition to the customary components of washing agents, contain 0 to 10% by weight of a quaternary ammonium compound and 1 to 30% by weight of a softener system which comprises 10 to 90% by weight of a tertiary amine and 90 to 10% by weight of a crystalline sheet-silicate of the formulaMe.sub.2 Si.sub.x O.sub.2x+1 .multidot. yH.sub.2 Oin which Me denotes an alkali metal ion or a proton, x denotes a number greater than 7, in particular from 7.5 to 23, and y denotes a number smaller than 7 x, in particular smaller than x. In the softener system, the tertiary amine is in a state of adsorption on the alkali metal silicate. The ammonium compounds, which are adsorbed on said silicate, produce a softening effect in the washing agent but on the other hand are compatible with anionic surfactants in the washing agent. produce a softening effect in the washing agent but on the other hand are compatible with anionic surfactants in the washing agent.Type: GrantFiled: May 2, 1985Date of Patent: May 20, 1986Assignee: Hoechst AktiengesellschaftInventors: Hans-Peter Rieck, Hans-Jurgen Kalz, Adolf May, Jochen M. Quack, Hans-Walter Bucking
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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
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Patent number: 4585641Abstract: This invention relates to crystalline gallosilicates having the following composition in terms of the mole ratios of the oxides:0.9.+-.0.25M.sub.2 /.sub.n O:Ga.sub.2 O.sub.3 :xSiO.sub.2 :yH.sub.2 O.zQwherein M is at least one cation having a valence n, x is at least 10, y/x is from 0 to 30, Q is a template used in the synthesis of the gallosilicate and z/x is 0-20, wherein the gallosilicate in the organic free hydrogen-form has an X-ray diffraction pattern substantially as set forth in Table A of this specification. The gallosilicates may be used, whether or not impregnated and/or ion-exchanged, admixed, supported or bound, for catalyzing a reaction selected from alkylation, dealkylation, dehydrocyclodimerization, aromatization, transalkylation, isomerization, dehydrogenation, hydrogenation, cracking, hydrocracking, cyclization, oligomerization, polymerization, conversion of carbon monoxide/hydrogen mixtures to hydrocarbons and dehydration reactions.Type: GrantFiled: May 15, 1985Date of Patent: April 29, 1986Assignee: The British Petroleum Company P.L.C.Inventors: Sami A. I. Barri, Dennis Young
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Patent number: 4582815Abstract: The present invention is directed to a method for extruding silica-rich solids. The method comprises mixing silica-rich solids with water in an alkali metal base or basic salt followed by mulling and extruding and subsequently drying the extrudate whereby the dried extrudate has a crush strength superior to that of the prior art. The silica-rich solids can be silica alone, zeolite alone or a mixture thereof. The alkali metal can be sodium hydroxide. The invention is also directed to a product which has a special attribute in that they have sufficient integrity to withstand treatments with acids so that it is now possible to steam, acid extract, or calcine such extrudates. The catalyst can be used in hydrocarbon conversions such as hydrocracking, isomerization, hydrogenation, dehydrogenation, polymerization, reforming, catalytic cracking, or catalytic hydrocracking.Type: GrantFiled: July 6, 1984Date of Patent: April 15, 1986Assignee: Mobil Oil CorporationInventor: Emmerson Bowes
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Patent number: 4581292Abstract: The present invention provides a synthetic amorphous zirconium-bonded silicate obtained by reacting, as main starting materials, a water-soluble alkali-metal silicate with an inorganic zirconyl salt and a mineral acid, in which zirconium is bonded to silica at the ratio of ZrO.sub.2 to SiO.sub.2 being 0.1 to 10 weight percent, which silicate is useful as a dentifrice base material and also as a filler for rubber.Type: GrantFiled: August 9, 1984Date of Patent: April 8, 1986Assignees: Lion Corporation, Taki Chemical Co., Ltd.Inventors: Shozo Shinpo, Tetsuo Fushino, Akihiro Hachijo, Shozo Ohtsu
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Patent number: 4581213Abstract: Crystalline sodium silicates having a sheet structure and an ion exchange capacity of 83-130 mmol of Na.sup.+ /mol of SiO.sub.2 are prepared by a method in which an aqueous reaction mixture which contains sodium silicate, has a molar ratio SiO.sub.2 /Na.sub.2 O of 3.9:1 to 15:1 and a molar ratio H.sub.2 O/(Na.sub.2 O+SiO.sub.2) of 3:1 to 80:1 and contains 0.01 to 30% by weight, relative to the amount of SiO.sub.2 in the reaction mixture employed, of seed crystals of the desired crystalline sodium silicate is prepared, the mixture is heated to temperatures of 160.degree. to 250.degree. C., the reaction is carried out at least until, in the X-ray diffraction pattern of a sample filtered off under suction and dried at 120.degree. C., the ratio of the intensity of the reflection at the interplanar spacing d.sub.1 =(20.+-.2).multidot.10.sup.-8 cm to the intensity of any reflection present at the interplanar spacing d.sub.2 =(15.5.+-.1.5).multidot.10.sup.Type: GrantFiled: January 2, 1985Date of Patent: April 8, 1986Assignee: Hoechst AktiengesellschaftInventor: Hans-Peter Rieck
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Patent number: 4581216Abstract: A crystalline aluminosilicate zeolite is obtained by stirring under heating an aqueous reaction mixture containing a silica source, an alumina source, an alkali source and an organic carboxylic acid.Type: GrantFiled: January 22, 1985Date of Patent: April 8, 1986Assignee: Toray Industries, IncorporatedInventors: Kazuyoshi Iwayama, Takao Kamano, Kuniyuki Tada, Takehisa Inoue
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Patent number: 4578258Abstract: A process for the preparation of a crystalline sheet-type alkali metal silicate in an aqueous medium is described, in which an acidic compound is added to an amorphous alkali metal silicate, or an alkali metal silicate dissolved in water, having a molar ratio M.sub.2 O/SiO.sub.2 (M=alkali metal) of 0.24 to 2.0, in an amount such that a molar ratio M.sub.2 O (unneutralized)/SiO.sub.2 of 0.05 to 0.239 is obtained. If required, the molar ratio SiO.sub.2 /H.sub.2 O is adjusted from 1:5 to 1:100 by dilution, and the reaction mixture is kept at a reaction temperature of 70.degree. to 250.degree. C. until the sheet-type alkali metal silicate has crystallized out.Type: GrantFiled: January 2, 1985Date of Patent: March 25, 1986Assignee: Hoechst AktiengesellschaftInventor: Hans-Peter Rieck
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Patent number: 4568654Abstract: A novel crystalline zeolite identified as zeolite ZSM-51 and its method of preparation is disclosed. The use of the material as a catalyst is also disclosed.Type: GrantFiled: August 13, 1984Date of Patent: February 4, 1986Assignee: Mobil Oil CorporationInventor: Ernest W. Valyocsik
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Patent number: 4565681Abstract: This invention relates to a new and useful improvement in synthesizing crystalline ZSM-5 zeolite and to use of said zeolite prepared in accordance herewith as a catalyst for hydrocarbon conversions. The synthesis utilizes dimethylethylpropylammonium ion as the directing agent.Type: GrantFiled: May 3, 1984Date of Patent: January 21, 1986Assignee: Mobil Oil CorporationInventor: Gunter H. Kuhl
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Patent number: 4564511Abstract: A method for preparing a molecular sieving metallosilicate is disclosed which comprises(A) providing a mixture comprising: water; an oxide of silicon source; a mineralizing agent and/or synthesis directing agent; and a heteropolymetallate of the formulaA.sub.a L.sub.l M.sub.m J.sub.z O.sub.y .dH.sub.Type: GrantFiled: November 16, 1984Date of Patent: January 14, 1986Assignee: The Standard Oil Company (Ohio)Inventors: Michael J. Desmond, Frederick A. Pesa
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Patent number: 4559213Abstract: There is disclosed a process for preparing a ZSM-12 crystalline zeolite wherein the organic template used in the synthesis has the formula: ##STR1## wherein n=4-10. The template, designated herein DABCO-C.sub.n -diquat, is obtained from a dihalide salt of the template or from a hydroxide thereof.Type: GrantFiled: September 17, 1984Date of Patent: December 17, 1985Assignee: Mobil Oil CorporationInventor: Gunter H. Kuhl
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Patent number: 4557815Abstract: The ratio of silica to alkali in silicate liquors is increased, for example to convert alkaline grades to neutral grades, by passing the liquors through an electrodialysis stack comprising alternating cation exchange membranes and bipolar membranes mounted between an anode and a cathode, the membranes forming a concentrating cell between the anion exchange side of the bipolar membrane and the adjacent cation exchange membrane and a diluting cell between the cation exchange side of the bipolar membrane and the adjacent cation exchange membrane, the method comprising passing the silicate liquor through the diluting cells in the stack and passing water or an aqueous solution through the concentrating cells, whereby the silicate liquor is caused to lose alkali metal ions to the concentrating liquor and receive hydrogen ions from the bipolar membranes.Type: GrantFiled: September 21, 1984Date of Patent: December 10, 1985Assignee: Imperial Chemical Industries PLCInventors: Graham W. Scott, James H. Steven
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Patent number: 4557858Abstract: The invention provides an electronically conductive tectosilicate which has, trapped within and forming part of its framework structure at the molecular or atomic level, colloidal particles of one or more electronically conducted species, which act to render the tectosilicate electronically conductive. The invention further provides a method of making such electronically conductive tectosilicate, wherein, for example, a zeolite is precipitated from the solution which has an electronically conductive species such as colloidal graphite in suspension therein, so that the colloidal particles of the electronically conductive species are trapped within and form part of the framework structure of the precipitate at the atomic or molecular level. The invention also extends to electronically conductive artifacts, such as electrodes for electrochemical cells, which are made from the electronically conductive tectosilicate by compacting the artifact from particles of the tectosilicate.Type: GrantFiled: March 14, 1983Date of Patent: December 10, 1985Assignee: Lilliwyte Societe AnonymeInventor: Roy C. Galloway
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Patent number: 4557916Abstract: Alkaline earth metal alumino silicates of the formula:(0.1-720)Me:(0.005-100)B.sub.2 O:Al.sub.2 O.sub.3 :(1.0-400)SiO.sub.2 :XH.sub.2 Owherein Me is an alkaline earth metal, B is an alkali metal, and X is an integer of 1 to 3, are amorphous very high structure absorbents. The products are prepared by reaction of a reactive clay with an alkaline earth metal or hydroxide.Type: GrantFiled: October 22, 1984Date of Patent: December 10, 1985Assignee: J. M. Huber CorporationInventor: Michael C. Withiam
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Patent number: 4557919Abstract: A process for producing a crystalline zeolite TPZ-12, which comprises maintaining a starting mixture at a temperature of at least 80.degree. C. for a period sufficient to produce zeolite crystals, said starting mixture consisting of(a) a substance capable of yielding silica under the reaction conditions,(b) a water-soluble alkali metal compound,(c) water, and(d) a diammonium compound represented by the following general formula ##STR1## wherein R.sub.1 and R.sub.2 are identical or different and each represents a hydrogen atom or an alkyl group having 1 to 4 carbon atoms, p and q are identical or different and each represents an integer of 4 or 5, n is 4, 5 or 6, and y represents an anion having a valence of m, and additionally, if desired,(e) a substance capable of yielding alumina under the reaction conditions,in the particular quantities.Type: GrantFiled: April 10, 1984Date of Patent: December 10, 1985Assignee: Teijin Petrochemical Industries Ltd.Inventors: Koji Sumitani, Tokuji Sakai, Yasuo Yamasaki, Tamio Onodera
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Patent number: 4556466Abstract: The ratio of silica to alkali in silicate liquors is increased, for example to convert alkaline grades to neutral grades, by passing the liquor through an electrodialysis stack comprising spaced ion-exchange membranes mounted between an anode and a cathode, the membranes forming cell triplets of a concentrating cell between an ion-exchange membrane and a fine cation exchange membrane, a diluting cell between the first cation exchange membrane and a second cation exchange membrane and a proton donor cell between the second cation exchange membrane and an adjacent anion-exchange membrane, the method comprising passing the silicate liquors through the diluting cells in the stack, passing water or an aqueous solution through the concentrating cells and passing an acidic solution through the proton donor cells whereby the silicate liquor is caused to lose alkali metal ions to the concentrating liquor and to receive hydrogen ions from the proton donor liquor.Type: GrantFiled: September 21, 1984Date of Patent: December 3, 1985Assignee: Imperial Chemical Industries plcInventors: Graham W. Scott, James H. Steven
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Patent number: 4556549Abstract: This invention relates to a method for preparing a synthetic porous crystalline aluminosilicate zeolite, characterized as zeolite ZSM-45. This crystalline material may have a molar ratio of silica to alumina of at least 8. This synthetic zeolite is analogous, in some respects, to the naturally occuring zeolite, levynite. The ZSM-45 zeolite is prepared with a cobalticinium directing agent. ZSM-45 exhibits a characteristic X-ray diffraction pattern.Type: GrantFiled: November 29, 1983Date of Patent: December 3, 1985Assignee: Mobil Oil CorporationInventor: Ernest W. Valyocsik
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Patent number: 4556550Abstract: A process is provided for achieving a high degree of exchange for zeolites, e.g., Zeolites F and W. After preparation of the ammonium form, the zeolite is contacted with a solution containing the desired metal cation while simultaneously maintaining the pH at between about 9.0 and 12.0 to provide a final product zeolite wherein the desired metal cation will correspond to at least about 0.5 of the total zeolitic cations.Type: GrantFiled: October 19, 1983Date of Patent: December 3, 1985Assignee: Union Carbide CorporationInventors: Ronald J. Ross, John D. Sherman
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Patent number: 4556465Abstract: The ratio of silicate to alkali in silicate liquors is increased, for example to convert alkaline grades to neutral grades, by passing the liquors through an electrodialysis stack comprising alternating anion exchange membranes and cation exchange membranes mounted between an anode and a cathode, the membranes being spaced apart to provide cells through which a fluid can be passed, the method comprising passing the silicate liquor through those cells having their anion exchange membranes on the anode side and passing water or an aqueous solution through the other cells, whereby the silicate liquor is caused to lose alkali metal ions.Type: GrantFiled: September 21, 1984Date of Patent: December 3, 1985Assignee: Imperial Industries plcInventors: Graham W. Scott, James H. Steven
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Patent number: 4552739Abstract: A novel method for preparing ZSM-12 utilizing diethyldimethylammonium cation in the forming solution.Type: GrantFiled: May 3, 1985Date of Patent: November 12, 1985Assignee: Mobil Oil CorporationInventor: Gunter H. Kuhl
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Patent number: 4542002Abstract: Silicate having high ion exchange capacity are obtained by reacting sepiolites with a base, preferably a strong base in the presence of a polar liquid at a temperature, preferably elevated, and for a period sufficient to increase the ion exchange capacity to at least 50 meq. per 100 g, more preferably at least 100 meq. per 100 g. In the preferred form, the reaction is carried out at above 100.degree. C. in an autoclave.Type: GrantFiled: February 28, 1983Date of Patent: September 17, 1985Assignee: Synthesis Engineering Ltd.Inventors: Avelino C. Corma, Amparo C. Mifsud, Joaquin P. Perez
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Patent number: 4539191Abstract: Sodium silicate solutions are prepared by dissolving sand in sodium hydroxide solution at a pressure of at least 100 psig and at a temperature of at least 130.degree. C. to produce a sodium silicate solution having a silica to sodium oxide molar ratio of between 2.4:1 and 2.8:1, and activating said sodium silicate solution by reaction with from about 50 to 200 ppm of alumina.Type: GrantFiled: November 7, 1983Date of Patent: September 3, 1985Assignee: J. M. Huber CorporationInventor: John A. Kostinko
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Patent number: 4539193Abstract: 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: May 23, 1984Date of Patent: September 3, 1985Assignee: Mobil Oil CorporationInventor: Ernest W. Valyocsik
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Patent number: 4537754Abstract: A new zeolite material designated EU-1 having a molar composition expressed by the formula:0.5 to 1.5 R.sub.2 O:Y.sub.2 O.sub.3 : at least 10 XO.sub.2 :0 to 100 H.sub.2 Owherein R is a monovalent cation or .sup.1 /n of a cation of valency n, X is silicon and/or germanium, Y is one or more of aluminum, iron, gallium or boron, and H.sub.2 O is water of hydration additional to water notionally present when R is H, and having an X-ray pattern substantially as set out in Tables 1 and 2 is prepared from a reaction mixture containing XO.sub.2 (preferably silica), Y.sub.2 O.sub.3 (preferably alumina) and a dicationic alkylated polymethylene diamine. The new zeolite is useful in catalytic processes, especially xylenes isomerization.Type: GrantFiled: June 11, 1981Date of Patent: August 27, 1985Assignee: Imperial Chemical Industries PLCInventors: John L. Casci, Barrie M. Lowe, Thomas V. Whittam
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Patent number: 4528172Abstract: The invention provides a process for the manufacture of zeolites of the ZSM-5 type by heating an aqueous solution or suspension containing a silicon dioxide source, alkali metal hydroxide and optionally an aluminum source until crystallization occurs. Furthermore, the solution or suspension contains an organic phosphorus compound which is selected from the group consisting of OPR.sup.1 R.sup.2 R.sup.3 and PR.sup.1 R.sup.2 R.sup.3, in which R.sup.1, R.sup.2 and R.sup.3, independently from one another, each are alkyl or alkoxy having each from 2 to 10 carbon atoms.Type: GrantFiled: October 11, 1983Date of Patent: July 9, 1985Assignee: Hoechst AktiengesellschaftInventors: Hans-Peter Rieck, Hans-Jurgen Kalz
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Patent number: 4528171Abstract: A synthetic zeolite material, designated zeolite EU-4, having a molar composition expressed by the formula:O to M.sub.2 O:aY.sub.2 O.sub.3 :at least 100 XO.sub.2 :0 to 35 H.sub.2 Owherein M is a monovalent cation or 1/n of a cation of valency n, a is from 0 to 9, X is silicon and/or germanium, Y is one or more of aluminum, iron, chromium, vanadium, molybdenum, arsenic, antimony, manganese, gallium or boron, and H.sub.2 O is water of hydration additional to water notionally present when M is H, and having a defined X-ray diffraction pattern is prepared from an aqueous reaction mixture containing the oxide XO.sub.2, optionally the oxide Y.sub.2 O.sub.3 and an alkyltrimethylammonium or dialkyldimethylammonium compound.Zeolite EU-4 is a useful catalyst for methanol conversion and the like.Type: GrantFiled: April 12, 1982Date of Patent: July 9, 1985Assignee: Imperial Chemical Industries, PLCInventors: John L. Casci, Barrie M. Lowe, Thomas V. Whittam
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Patent number: 4520001Abstract: The process for producing a clear solution of alkali metal silicate having an SiO.sub.2 /alkali metal oxide weight ratio of 2.5 or less which comprises passing an aqueous solution of an alkali metal hydroxide through a bed of crystallized silica having an average particle size of between about 0.1 mm and 2 mm formed in the bottom of a vertical tubular reactor without mechanical agitation, said silica and alkali metal hydroxide being fed from the top of the reactor, and recovering the resulting clear solution of alkali metal silicate from the bottom of the reactor.Type: GrantFiled: April 6, 1983Date of Patent: May 28, 1985Inventors: Jean Metzger, Henri Lecouls, Philippe Colombe, Jean Wojcik
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Patent number: 4499062Abstract: A process for the hydrothermal fusion of aluminum silicate and alkali aluminum silicates with aqueous sodium hydroxide solution under pressure and at elevated temperatures in the presence of soluble silicates, in which an aqueous solution containing from about 20 to about 50% by weight of NaOH is mixed with aluminum silicates and/or alkali aluminum silicates, and with a hydrothermally fusible silicate component, wherein the ratio by weight of SiO.sub.2 to Al.sub.2 O.sub.3 in the mixture amounts to at least 30:1 and the ratio by weight of SiO.sub.2 to Na.sub.2 O amounts to at least 1.5:1, and the mixtures are reacted at temperatures of from about 180.degree. to about 250.degree. C. and under the saturated steam pressures corresponding to those temperatures. The resulting sodium silicate solution, which contains the dissolved aluminum, is then separated off.Type: GrantFiled: May 27, 1983Date of Patent: February 12, 1985Assignee: Henkel Kommanditgesellschaft auf AktienInventors: Peter Christophliemk, Rudolf Novotny, Jurgen von Laufenberg, Josef Sadlowsky
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Patent number: 4496528Abstract: The invention relates to the preparation of the zeolite ZK-5 from a starting zeolite selected from the group consisting of the zeolites P (Cl), P' (Cl), Q (Br) and Q' (Br).In accordance with the invention, the barium ions contained in the starting zeolite are extracted therefrom by means of a barium-binding agent selected from the group consisting of precipitating agents which form with the barium ions a compound that precipitates, and of complexing agents which form with the barium ions a barium complex.The zeolite ZK-5 obtained may be used in the separation or cracking of hydrocarbons.Type: GrantFiled: March 29, 1983Date of Patent: January 29, 1985Assignee: Compagnie Francaise de RaffinageInventors: Michel Bourgogne, Jean-Louis Guth, Georges Szabo, Raymond Wey
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Patent number: 4482531Abstract: There is disclosed a process for preparing a ZSM-12 crystalline zeolite wherein the organic template used in the synthesis has the formula: ##STR1## wherein n=4,5,6 or 10. The template, designated herein DABCO-C.sub.n -diquat, is obtained from a dihalide salt of the template or from a hydroxide thereof.Type: GrantFiled: April 29, 1983Date of Patent: November 13, 1984Assignee: Mobil Oil CorporationInventor: Guenter H. Kuehl
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Patent number: 4481173Abstract: The alkali metal content of zeolite ZSM-11 in its as-synthesized form is reduced by crystallizing the zeolite from a solution containing a source of benzyltrimethyl ammonium ions.Type: GrantFiled: November 22, 1982Date of Patent: November 6, 1984Assignee: Mobil Oil CorporationInventor: Pochen Chu
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Patent number: 4481177Abstract: An improved process for preparing ZSM-22 zeolite is disclosed and claimed. The process comprises preparing a reaction mixture comprised of sources of an alkali or alkaline earth metal, alumina, silica, organic promoter and water, and having the following composition, in terms of mole ratios of oxides:SiO.sub.2 /Al.sub.2 O.sub.3 =20 to .infin.H.sub.2 O/SiO.sub.2 =10 to 100OH.sup.- /SiO.sub.2 =0 to 1.0M.sup.+ /SiO.sub.2 =0 to 2.0RN/SiO.sub.2 =0.01 to 2.0wherein RN is a functional group of a heterocyclic organic compound containing one or more four (4) to ten (10) member, saturated or unsaturated, non-fused rings, wherein the hetero atoms are the same or different, and they are oxygen, phosphorus or nitrogen, an alkyl and/or alkene derivative of the heterocyclic organic compound, wherein the alkyl and/or alkene groups contain one (1) to ten (10) carbon atoms, or an organic or inorganic salt of the heterocyclic organic compound or its alkyl or alkene derivative, and M is an alkali or alkaline earth metal, e.g.Type: GrantFiled: December 9, 1982Date of Patent: November 6, 1984Assignee: Mobil Oil CorporationInventor: Ernest W. Valyocsik
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Patent number: 4478796Abstract: There is provided a process for replacing the magnesium oxide portion of a nature magnesium silicate with sodium oxide thereby to form sodium silicate which comprises melting a natural magnesium silicate and sodium carbonate at a temperature of from 1100.degree. to 1350.degree. C. until a clear melt is obtained, the molar ratio of sodium oxide derived from the sodium carbonate per mole of silica contained in the natural magnesium silicate being from 4:1 to 7:1, quenching and extracting said clear melt with water and separating the insoluble magnesium oxide from the solution containing predominantly sodium silicate and sodium hydroxide.Type: GrantFiled: February 17, 1983Date of Patent: October 23, 1984Assignee: Societe Nationale de LiamianteInventors: Jean M. Lalancette, Jean P. Drolet
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Patent number: 4472366Abstract: A method of synthesizing a crystalline aluminosilicate zeolite from a reaction mixture containing a base, silica, alumina and water, wherein an alkali metal compound and an amide compound are concurrently used as said base.Type: GrantFiled: December 1, 1982Date of Patent: September 18, 1984Assignee: Catalysts & Chemicals Industries Co., Ltd.Inventors: Hiroshi Takahashi, Hiromi Nakamoto
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Patent number: 4462971Abstract: Crystalline metal silicates and metal borosilicate compositions exhibit useful catalytic properties when the reaction mixture from which they are prepared includes a metal whose oxide precipitates at a pH above 7 and an amount of urea or other compound which upon hydrolysis releases ammonia. The precipitated metal hydroxide is incorporated into the crystalline composition as it forms. These compositions exhibit the X-ray pattern of a ZSM-5 zeolite and have an aluminum content of less than 100 wppm and a composition expressed in terms of its oxides as follows:(0.2-80)R.sub.(2/n) O: (0.1-20) M.sub.(2/m) O: (0-40)B.sub.2 O.sub.3 : 100 SiO.sub.2 :(0-200)H.sub.2 Owhere R is tetramethyl ammonium cation, ammonium cation, hydrogen cation, an alkali metal cation, metal cation or mixtures thereof, n is the valence of R, M is a metal whose hydroxide precipitates at a pH above 7 and m is the valence of said metal. These crystalline silicates and borosilicates are usefully employed as catalysts in hydrocarbon conversions.Type: GrantFiled: December 29, 1982Date of Patent: July 31, 1984Assignee: National Distillers and Chemical CorporationInventors: James A. Hinnenkamp, Vernon V. Walatka, Jr.
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Patent number: 4430314Abstract: A method of preparing zeolite ZSM-5 type crystals and mixtures thereof which comprises crystallizing the substantially pure zeolite material from a silica and, optionally, alumina gel mixture in the presence of organic nitrogen-N-oxides and the products produced thereby, thermally or unthermally treated.Type: GrantFiled: April 5, 1982Date of Patent: February 7, 1984Assignee: Mobil Oil CorporationInventors: Costandi A. Audeh, William J. Reagan
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Patent number: 4423021Abstract: A new porous silico-crystal, a method of making same and the use thereof in catalytic conversion of organic compounds. The new product has a composition, expressed in terms of moles of anhydrous oxides per 100 moles of silica as follows:(0 to 15)RN : (0 to 1.5)M.sub.2/n O : (0-2)Al.sub.2 O.sub.3 : (100)SiO.sub.2wherein M is at least one cation having a valence n, RN is a C.sub.1 -C.sub.20 organic compound, having at least one amine functional group of pK.sub.a .gtoreq.7 and wherein the zeolite is characterized by the distinctive X-ray powder diffraction pattern shown in Table I. The new silico-crystal is prepared from a reaction mixture comprising a source of silica, C.sub.1 -C.sub.20 organic compounds, as defined above, with or without a source of alumina, and water.Type: GrantFiled: November 18, 1980Date of Patent: December 27, 1983Assignee: Mobil Oil CorporationInventors: Louis D. Rollmann, Ernest W. Valyocsik
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Patent number: 4420467Abstract: A synthetic zeolite material, designated zeolite Nu-5, having a molar composition expressed by the formula; 0.5 to 1.5 R.sub.2 O: Y.sub.2 O.sub.3 : at least 10 XO.sub.2 : 0 to 2000 H.sub.2 O wherein R is a monovalent cation or 1/n of a cation of valency n, X is silicon and or germanium, Y is one or more of aluminium, iron, chromium, vanadium, molybdenum, arsenic, manganese, gallium or boron, and H.sub.2 O is water of hydration additional to water notionally present when R is H, and having a defined X-ray diffraction pattern. Zeolite Nu-5 is a useful catalyst.Type: GrantFiled: December 17, 1981Date of Patent: December 13, 1983Assignee: Imperial Chemical Industries PLCInventor: Thomas V. Whittam
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Patent number: H262Abstract: A method of and system for removing silicon from a high temperature liquid sodium coolant system for a nuclear reactor. The sodium is cooled to a temperature below the silicon saturation temperature and retained at such reduced temperature while inducing high turbulence into the sodium flow for promoting precipitation of silicon compounds and ultimate separation of silicon compound particles from the liquid sodium.Type: GrantFiled: November 25, 1983Date of Patent: May 5, 1987Assignee: The United States of America as represented by the United States Department of EnergyInventors: Wayne H. Yunker, David W. Christiansen