By Precipitating Or Gelling From Silicate Solution Patents (Class 423/333)
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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: 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: 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: 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: 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: 4537758Abstract: A method of preparing a highly siliceous porous crystalline material related to the zeolite ZSM-12 having a composition, in terms of mole ratios of oxides, after dehydration, as follows:(1.0.+-.0.4)M.sub.2 /.sub.n O.multidot.Al.sub.2 O.sub.3 .multidot.(20-.infin.)SiO.sub.2,wherein M is at least one cation having a valence n, and characterized by an x-ray diffraction pattern whose values are set forth in Table 1 of the specification.Type: GrantFiled: March 19, 1984Date of Patent: August 27, 1985Assignee: Mobil Oil CorporationInventors: Pochen Chu, Guenter H. Kuehl
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Patent number: 4537866Abstract: A method of preparing a silica-containing composition from a lithium silicate sol is disclosed. The compositions are prepared by heating shaped particles of lithium silicate sol to a temperature of about 70.degree. C. or more in the absence of a gelling agent and thereafter subjecting the particles to a washing step to remove lithium therefrom. By means of the novel method it is possible to prepare silica-containing compositions which are suitable as catalyst and/or adsorbent supports.Type: GrantFiled: March 29, 1984Date of Patent: August 27, 1985Assignee: UOP Inc.Inventor: Jean-Pierre Gilson
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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: 4503158Abstract: An at least double silicate of an alkali metal and at least one other metal is prepared by interreacting (i) an aqueous solution of an alkali metal silicate and (ii) a solution of an oxide of such at least one other metal, or salt thereof, in the presence of (iii) a water-miscible polar organic liquid, whereby said at least double silicate is suspended in the organic reaction medium in insoluble and finely divided form. The separated product is an admirable glass-former.Type: GrantFiled: April 13, 1983Date of Patent: March 5, 1985Assignee: Rhone-Poulenc IndustriesInventor: Christian Richard
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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: 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: 4452907Abstract: Crystalline aluminosilicates having a silica to alumina molar ratio greater than 12 are produced by mixing a source of silica, a source of alumina, a source of alkali metal, water and a source of ammonium ions, e.g. ammonia or an ammonium salt, in the absence of an alcohol or alkylene oxide, in the molar proportions (expressed in the case of the silica and alumina sources in terms of the equivalent moles of the oxide, in the case of the alkali metal source in terms of the equivalent moles of the hydroxide (MOH) and in the case of the source of ammonium ions in terms of free ammonia):SiO.sub.2 : Al.sub.2 O.sub.3 greater than 12:1MOH: Al.sub.2 O.sub.3 in the range from 1:1 to 20:1SiO.sub.2 : NH.sub.3 in the range from 1:1 to 200:1H.sub.2 O: MOH in the range from 30:1 to 300:1and maintaining the composition at elevated temperature, such as 120.degree. to 210.degree. C. for a period such that crystallization occurs, typically greater than 4 hours.Type: GrantFiled: December 28, 1982Date of Patent: June 5, 1984Assignee: The British Petroleum Company LimitedInventors: William J. Ball, David G. Stewart
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Patent number: 4452769Abstract: A method of preparing a zeolite ZSM-12 type crystal which comprises crystallizing substantially pure ZSM-12 from a silica and optimally alumina gel mixture in the presence of a methyltriethylammonium cation, and the ZSM-12 product produced thereby.Type: GrantFiled: February 17, 1981Date of Patent: June 5, 1984Assignee: Mobil Oil CorporationInventors: Pochen Chu, Guenter H. Kuehl
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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: 4329328Abstract: Sodium zinco/stanno/titano-silicate is synthesized by mixing a concentrated aqueous sodium zincate, stannate or titanate solution with a source of silica (e.g. powdered glass or sodium metasilicate solution) in the ratio 60 g sodium silicate to sodium zincate equivalent to 8.1 g zinc oxide, keeping the temperature at 40.degree. C. for 1/2 hour, diluting threefold with water of 20.degree. C., allowing a precipitate to form overnight, and filtering and drying the residue at 110.degree. C.The resulting sodium zincosilicate may be used in its own right as a water softener or may be converted by cation exchange into any other desired zincosilicate.Type: GrantFiled: October 16, 1980Date of Patent: May 11, 1982Assignee: National Research Development CorporationInventors: Patrick McAnespie, Alan Dyer, Bharati J. Mehta
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Patent number: 4299808Abstract: There are provided crystalline chromosilicates, their methods of preparation, and process uses. A first crystalline chromosilicate comprises a molecular sieve material providing a specific X-ray diffraction pattern and having the following composition in terms of mole ratios of oxides:0.9.+-.0.2 [WR.sub.2 O+(1-W)M.sub.2/n O]: Cr.sub.2 O.sub.3 : YSiO.sub.2 : ZH.sub.2 O,wherein R is an alkylammonium cation, M is at least one cation having a valence of n, Y is a value within the range of about 4 to about 500, Z is a value within the range of about 0 to about 160, and W is a value that is greater than or equal to 0 and less than or equal to 1. A second crystalline chromosilicate comprises a molecular sieve material providing a specific X-ray diffraction pattern and having the following composition in terms of mole ratios of oxides:0.9.+-.0.2 M.sub.2/n O: Cr.sub.2 O.sub.3 : YSiO.sub.2 : ZH.sub.Type: GrantFiled: August 23, 1979Date of Patent: November 10, 1981Assignee: Standard Oil Company (Indiana)Inventor: Marvin R. Klotz
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Patent number: 4133665Abstract: The present invention is concerned with the production of sodium and/or potassium hydrosilicate glass bodies. The basis of the invention resides in the hydration of anhydrous sodium and/or potassium silicate glass bodies in aqueous alcohol solutions to impart enhanced mechanical strength and thermoplastic properties thereto. The hydrating process, which permits close control to be maintained over the water content absorbed in the glass, can be carried out in liquid solutions of water and relatively short chain, i.e. up to about five carbon atoms, aliphatic alcohols or in gaseous atmospheres of such solutions. An ion exchange reaction of Li.sup.+ ions or protons with Na.sup.+ and/or K.sup.+ ions can be promoted at temperatures above the transformation range of the hydrated glass, and an exchange of K.sup.+ ions for Na.sup.+ and/or Li.sup.+ ions at temperatures below the transformation range.Type: GrantFiled: September 1, 1977Date of Patent: January 9, 1979Assignee: Corning Glass WorksInventors: Roger F. Bartholomew, William L. Haynes, Leon M. Sanford
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Patent number: 4124471Abstract: A novel method of controlling electrodialytically produced silica sol particle size and concentration comprising effecting electrodialysis of an alkali metal silicate anolyte in an electrodialysis cell with a cation permselective membrane separating the anolyte and the catholyte while adding alkali metal silicate solution to the anolyte to maintain the desired pH whereby a silica sol with increasing particle size is formed and when the silica sol has reached the desired particle size, continuing electrodialysis with addition of an alkali metal hydroxide solution to control the pH until the silica sol has the desired concentration.Type: GrantFiled: August 22, 1977Date of Patent: November 7, 1978Assignee: Diamond Shamrock CorporationInventors: Donald F. Lieb, Thomas T. Sugano
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Patent number: 4054537Abstract: This invention provides a process for synthesizing compositions containing trioctahedral smectite-type clays which contain fluorine within their layer lattices. In particular, the invention provides a process for synthesizing compositions having mole ratios of Li, Na, Mg and Si, expressed as oxides, and F of:aLi.sub.2 O : bNa.sub.2 O : cMgO : dF : 8SiO.sub.2 (I)where 0.ltoreq.a<1.2, 0.ltoreq.b<0.6, 4.75.ltoreq.c<7, 0<d<4, o.ltoreq.a+b<1.4, and 5.5<a+b+c<8, and where c.gtoreq.6 when a+ b= 0.Type: GrantFiled: August 2, 1976Date of Patent: October 18, 1977Assignee: N L Industries, Inc.Inventors: Alan C. Wright, Joseph Paul Rupert
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Patent number: 4040974Abstract: This invention provides a gellant which is a synthesized complex of a fluorine-containing trioctahedral smectite-type clay and an amorphous occluded phase selected from the group consisting of lithium hydroxide, sodium hydroxide, magnesium hydroxide, lithium oxide, sodium oxide, magnesium oxide, and mixtures thereof, the gellant having mole ratios of Li, Na, Mg and Si, expressed as oxides, and F of:aLi.sub.2 O:bNa.sub.2 O:cMgO:dF:8SiO.sub.2 (I)where 0.25.ltoreq.a<1.1, 0.ltoreq.b<0.60, 4.75<c<5.85, 0.5<d.ltoreq.3.5, 0.60.ltoreq.a+b<1.25, and 6.0 <a+b+c<6.65.Type: GrantFiled: April 26, 1976Date of Patent: August 9, 1977Assignee: N L Industries, Inc.Inventors: Alan C. Wright, Joseph Paul Rupert
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Patent number: 4029736Abstract: Processing of pearlite by treating the same with an alkaline solution having a concentration of 40-140 g/l taken in an amount which brings the ratio of the liquid and solid phases to (0.7-1.5) : 1 and then separating by filtration the water glass, obtained in the process of heat treatment, from the residue formed.Type: GrantFiled: June 7, 1973Date of Patent: June 14, 1977Inventor: Garegin Sarkisovich Melkonian
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Patent number: 3998751Abstract: There is disclosed a method for the preparation of an oxidant-containing solid which is useful as an antiseptic agent, bleaching agent, oxidizing agent, etc. The solid, which can be prepared in a varied degree of water solubility, is prepared by reacting, in aqueous solution an alkali metal silicate with an oxidant which can be hydrogen peroxide or an alkali metal hypohalite. When a hypohalite is used as the oxidant, the resultant solid can be prepared in a varied degree of water solubility. Typically, a solution of sodium silicate is admixed with a solution of sodium hypochlorite, resulting in the formation of a voluminous, white precipitate that can be separated by filtration, decanting and the like, to obtain a solid containing the hypochlorite. The water solubility of this solid can be readily controlled by progressive dehydration of the solid, resulting in increasing water insolubility of the solid.Type: GrantFiled: October 21, 1974Date of Patent: December 21, 1976Inventor: William Bruce Murray
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Patent number: 3956467Abstract: An improved method for producing alkalimetal polysilicates is disclosed. The polysilicates are produced by hydrothermally reacting an aqueous dispersion of finely-divided silica and an alkali metal hydroxide. The synthesized reaction mixture is then spray dried with the solid product then being fractured and pulverized. The fractured particles are thereafter pelletized and dried in a fluidized bed to produce a product having predetermined characteristics or properties. The product can be used in adhesives, in the production of silica gel, in textiles and the like. However, their use as builders in detergents and in combination with known anionic, nonionic and amphoteric surface active compounds (surfactants) is disclosed as being particularly advantageous.Type: GrantFiled: June 7, 1974Date of Patent: May 11, 1976Inventor: Orlando L. Bertorelli