By Precipitating Patents (Class 423/339)
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Patent number: 4900529Abstract: ZSM-5 crystallites are produced with very low levels of blocking tetrapropyl ammonium ions (Q). The reaction mixture contains sources of silica, soda, alumina and trace amounts of Q ions as nucleation agents. Because the crystallites as synthesized from the aqueous medium exhibit only a very small fraction of blocking cations, there is always a diffusion path for the hydrated sodium ions to be exchanged without the need of prior removal of the blocking cations by calcination or otherwise. The small size crystallites can be exchanged, blended with other materials, and formed into catalyst particles. The silica to alumina ratio can be varied and when no aluminum is added, silicalite may be formed. The systhesis can be done in 24 hours or less.Type: GrantFiled: December 23, 1985Date of Patent: February 13, 1990Assignee: W. R. Grace & Co.-Conn.Inventors: Moises G. Sanchez, Charles C. Chang, Norman R. Laine, Sandra M. Waters
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Patent number: 4885149Abstract: A process for preparing silica comprising:(a) acidifying a basic aqueous solution containing silicate ions and molybdate ions to produce silicomolybodic acid;(b) adding to the acidified solution an organic base to precipitate a silicomolybdate; and,(c) heating the resulting precipitate to drive off volatile components and leave a purified form of silica is disclosed. The process is particularly useful for producing purified silica from dilute aqueous media.Type: GrantFiled: December 9, 1987Date of Patent: December 5, 1989Assignee: Canadian Patents and Development LimitedInventors: Anthony S. W. De Freitas, Archibald W. McCulloch, Alister G. McInnes
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Patent number: 4880574Abstract: Adsorbents comprising partially dried amorphous silica hydrogels having a moisture content of at least about 25 wt % and an average pore diameter of about 60 Angstroms or less are useful in processes for the removal of trace contaminants, specifically phospholipids and associated metal ions, from glyceride oils. Treatment of the partially dried hydrogels with organic acid increases their adsorption capacity for these trace contaminants.Type: GrantFiled: November 24, 1986Date of Patent: November 14, 1989Assignee: W. R. Grace & Co.-Conn.Inventor: William A. Welsh
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Patent number: 4874594Abstract: Precipitation silicas, in the form of aggregates as shown in FIG. 1, having a mean projected area of the aggregates which is higher than about 8,000 nm.sup.2 and preferably is higher than about 15,000 nm.sup.2. The present invention also concerns a process for the production of precipitation silica by maintaining a constant-volume reaction medium to provide suitable colloids of silica, reacting the colloids with an electrolyte and consolidating the resulting product by the addition of a solution of silicate and an acidifying agent to obtain a precipitation silica.Type: GrantFiled: August 5, 1987Date of Patent: October 17, 1989Assignee: Rhone-Poulenc Specialites ChimiquesInventor: Yvonick Chevallier
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Patent number: 4861572Abstract: An improved process for the manufacture of a metal oxide is disclosed. In the process wherein a hydrolyzable organometallic compound is hydrolyzed by an alkaline hydrolyzing agent in an alkaline organic solvent, and thereafter, the metal oxide is formed by a condensation reaction of a metal hydroxide resulting from the hydrolysis of the organometallic compound, the improvement comprises feeding the organometallic compound and the hydrolyzing agent into the organic solvent so that a concentration of the hydrolyzed compound is initially above a critical level of supersaturation, and thereafter, is maintained in a range from above an upper limit of solubility to the critical level of super-saturation. According to the above process, the metal oxide can be obtained in the form of a powder material with a uniform particle size distribution.Type: GrantFiled: December 24, 1987Date of Patent: August 29, 1989Assignee: Kabushiki Kaisya AdvanceInventors: Yoshihisa Sugoh, Yasuo Ochi
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Patent number: 4857289Abstract: Precipitated silicas which have the following physicochemical characteristics, depending on the manner in which they are milled:______________________________________ Pendulum roller mill Jet mill ______________________________________ BET m.sup.2 /g 15-110 15-110 surface area Tamped g/l 150-750 90-650 den- sity Cu abrasion in 10% mg 5-30 5-30 strength glycerol dispersion Lightness % 86-96 90-96 value Particle size dis- as in FIG. 1 as in FIG. 2 tribution curve determined by a Coulter Counter "ALPINE screen retain- % by <1.5 <0.1 ings" >63 .mu.m weight Viscosity of a 30% mPa.s 30,000 to 60,000 strength dispersion in a 1:1 glycerol/water mixture (Brookfield RTV, Sp5) ______________________________________are prepared by diluting a precipitated silica original suspension obtained according to German Published Application DAS 1,467,019 and simultaneously adding alkali metal silicate solution, sulfuric acid and water while keeping the pH constant between 7 and 9.Type: GrantFiled: May 5, 1988Date of Patent: August 15, 1989Assignee: Degussa AktiengesellschaftInventors: Peter Nauroth, Robert Kuhlmann, Gunter Turk, Adam Becker
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Patent number: 4857290Abstract: This invention provides a process for producing silica from silica sol which comprises preparing an acidic silica sol applied with a hydrogen peroxide treatment from an aqueous solution of alkali silicate, purifying the acidic silica sol by using a cationic exchange resin after pH adjustment and preparing silica from the silica sol obtained by neutralizing the thus purified acidic silica sol, that is, a production process for highly pure silica capable of removing, Ti as much as possible in the same manner as impurities such as Fe and Al.Type: GrantFiled: August 8, 1988Date of Patent: August 15, 1989Assignee: Moses Lake Industries, Inc.Inventor: Shumpei Shimizu
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Patent number: 4851036Abstract: There is disclosed a process and an apparatus for beneficiating a mineral ore, such as phosphate-containing ore, in a substantially vertical column. The feed subjected to the benefication preferably has a particle size of less than 20 mesh. The feed is introduced into the column, containing at least one baffle, into which there is also introduced a gas at the bottom portion thereof and a liquid through at least one column inlet at the top of the column. The baffle and the rates of introduction of the feed, the gas, and the liquid are such as to create relatively high turbulence conditions within the column. The enriched, beneficiated product is removed at the top of the column, while the waste products, such as silica-containing material, in the case of a phosphate ore, are recovered at the bottom of the column.Type: GrantFiled: September 18, 1987Date of Patent: July 25, 1989Assignee: Mobil Oil CorporationInventors: Robert J. Anthes, Ross A. Kremer, Susanne Von Rosenberg
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Patent number: 4842837Abstract: A process for producing fine spherical silica, comprising a step of hydrolyzing an alkoxysilane in a mixed solution comprising water and alcohol and containing an alkaline catalyst, wherein the amount of said alkaline catalyst is 0.5 to 10 in molar ratio to the alkoxysilane used, the concentration of water in said mixed solution of water and alcohol in 5 to 20 mol/lit., and the reaction temperature for said hydrolysis is 30.degree. C. or more.According to this process, there can be obtained highly monodisperse spherical silica containing only a very small amount of impurities and having a particle size of 100 nm or less.Type: GrantFiled: September 18, 1987Date of Patent: June 27, 1989Assignee: Shin-Etsu Chemical Co., Ltd.Inventors: Takaaki Shimizu, Toshihiro Okon
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Patent number: 4842838Abstract: Precipitation silicas, in the form of aggregates as shown in FIG. 1, having a mean projected area of the aggregates which is higher than about 8,000 nm.sup.2 and preferably is higher than about 15,000 nm.sup.2. The present invention also concerns a process for the production of precipitation silica by maintaining a constant-volume reaction medium to provide suitable colloids of silica, reacting the colloids with an electrolyte and consolidating the resulting product by the addition of a solution of silicate and an acidifying agent to obtain a precipitation silica.Type: GrantFiled: January 16, 1987Date of Patent: June 27, 1989Assignee: Rhone-Poulenc Specialites ChimiquesInventor: Yvonick Chevallier
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Patent number: 4810415Abstract: High purity silica powder formed from a sol-gel process is made from a quantity of an industrial grade hydrolizable silicon organometallic substance mixed with a quantity of an industrial grade organic solvent miscible in said organometallic substance and with a quantity of an acidified water having a pH less than 2 to form a solution. The solution is heated, then dried to form a gel, milled, and calcined to form the pure silica powder and the pure powder used to form encapsulated micro-miniature circuits.Type: GrantFiled: September 10, 1986Date of Patent: March 7, 1989Assignee: Dresser Industries, Inc.Inventors: Howard M. Winkelbauer, Glenn A. Moore
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Patent number: 4808397Abstract: A process for preparing spheroid particles of oxide compounds, having an average diameter of smaller than 3 microns. An emulsion is prepared of a hydrolyzable liquid oxide compound in a perfluoropolyether, the emulsion is reacted with water, water vapor or with a mixture, in any ratio, of water with a liquid miscible or immiscible with water so as to form an oxide hydrate which is recovered dried and calcined. Oxide compounds include oxides of Ti, Al, Zr, Si or B.Type: GrantFiled: July 27, 1987Date of Patent: February 28, 1989Assignee: Montedison S.p.A.Inventors: Enrico Albizzati, Emiliano M. Ceresa, Luciano Zaninetta
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Patent number: 4806329Abstract: A method of producing synthetic silica which is characterized by hydrolyzing a tetraalkoxysilane under a basic condition in the presence of an ammonium salt.Type: GrantFiled: September 4, 1986Date of Patent: February 21, 1989Assignee: Tama Chemicals Co., Ltd.Inventors: Toshitsura Cho, Mamoru Yoshizako
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Patent number: 4778667Abstract: This invention relates to novel silica spheroids and to their production by a phase separation technique in which an aqueous alkaline stabilized silica sol and an aqueous solution of a non-adsorbing polymer are mixed and acidified to produce the new silica spheroids.Type: GrantFiled: December 2, 1986Date of Patent: October 18, 1988Assignee: Unilever Patent Holdings B.V.Inventors: Michael J. Garvey, Ian C. Griffiths
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Patent number: 4775520Abstract: Highly monodispersed nonporous spherical SiO.sub.2 particles are prepared having mean particle diameters between 0.05 and 10 .mu.m with a standard deviation of not more than 5% and a method for the preparation of such particles. The particles can be produced by a two step process wherein first a sol of primary particles is prepared by hydrolytic polycondensation of tetraalkoxysilanes in an aqueous/alcoholic ammoniacal medium. The SiO.sub.2 particles are then converted to the desired particle size by a continuous measured addition of tetraalkoxysilane or organotrialkoxysilane controlled by the extent of the reaction. The SiO.sub.2 particles produced by this process are particularly useful as sorption material in chromatography.Type: GrantFiled: September 25, 1986Date of Patent: October 4, 1988Assignee: Merck Patent Gesellschaft mit Beschrankter HaftungInventors: Klaus Unger, Herbert Giesche, Joachim Kinkel
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Patent number: 4756903Abstract: Silica base material for dentifrice having excellent transparency, prolonged stability and desired abrasiveness, has a specific surface area of 270-500 m.sup.2 /g as measured by BET method and 5-60 m.sup.2 /g by CTAB method, gives virtually amorphous X-ray diffraction pattern after firing at 1100.degree. C., and has a refractive index of 1.455-1.470. This base material can be prepared by reacting an alkali metal silicate solution with hydrochloric acid or sulfuric acid in the presence of an electrolyte, controlling the ratio of the rate of addition of chloride ion or sulfate ion to be at least 3:2 between the acidification stage in which the pH at the completion of the reaction is brought to 3.5 or less, and the silica crystallization stage in which the pH of the reaction system if brought to 10.0, and carrying out the acidification stage within 30 minutes.Type: GrantFiled: February 19, 1987Date of Patent: July 12, 1988Assignee: Taki Chemical Co., Ltd.Inventors: Shinpo Shozo, Fushino Tetsuo, Hachijo Akihiro, Ohtsu Shozo
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Patent number: 4755369Abstract: There is provided a process for producing ultrafine particles by preparing one or more than one kind of alkoxide of a metal which is a component of the desired ultrafine particles, and subsequently hydrolyzing or heating said alkoxide. For the production of ultrafine particles of ruthenium oxide and/or metallic ruthenium, which are used as a raw material of thick film resistors, a ruthenium compound is reacted with an alkali metal alkoxide to give a ruthenium alkoxide and it is hydrolyzed or heated. For the production of a low-melting glass (including lead oxide), which is used as a sintering assistant or easy-to-sinter powder, at least three kinds of compounds (alkoxides or sols) including a lead alkoxide are reacted with one another and the resulting reaction product is hydrolyzed.Type: GrantFiled: March 13, 1986Date of Patent: July 5, 1988Assignee: Research Development Corporation of JapanInventor: Ozaki Yoshiharu
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Patent number: 4752458Abstract: A method of preparing spherical microparticles of silica comprising adding an acid solution to a silicate solution before or after addition of an alkali metal alginate, ammonium alginate, starch, gelatin, pectin or mixtures thereof. The microparticles can be used to prepare macroporous materials having a controlled pore structure.Type: GrantFiled: February 11, 1987Date of Patent: June 21, 1988Inventor: Eric Robinson
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Patent number: 4752459Abstract: A process for the preparation of at least one porous oxide or hydroxide body comprises:(i) adding at least one body comprising a sol of the oxide or hydroxide to a fluid freezing medium; and(ii) raising the temperature of the solid, quenched sol so that solvent nucleation occurs, resulting in the formation of crystals of the dispersion medium, and the dispersion medium melts thereby leaving one or more porous oxide or hydroxide bodies.Type: GrantFiled: March 27, 1986Date of Patent: June 21, 1988Inventor: Duncan S. Perrer
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Patent number: 4738838Abstract: Silica base material for dentifrice having excellent transparency, prolonged stability, and desired abrasiveness; has a specific surface area of 270-500 m.sup.2 /g as measured by BET method and 5-60 m.sup.2 /g by CTAB method, gives virtually amorphous X-ray diffraction pattern after firing at 1100.degree. C., and has a refractive index of 1.455-1.470. This base material can be prepared by reacting an alkali metal silicate solution with hydrochloric acid or sulfuric acid in the presence of an electrolyte, controlling the ratio of the rate of addition of chloride ion or sulfate ion to be at least 3:2 between the acidification stage in which the pH at the completion of the reaction is brought to 3.5 or less, and the silica crystallization stage in which the pH of the reaction system if brought to 10.0, and carrying out the acidification stage within 30 minutes.Type: GrantFiled: September 11, 1986Date of Patent: April 19, 1988Assignee: Taki Chemical Co., Ltd.Inventors: Shozo Shinpo, Tetsuo Fushino, Akihiro Hachijo, Shozo Ohtsu
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Patent number: 4738839Abstract: Crystalline precipitated silica is produced by hydrolyzing silicon tetrachloride in the presence of fluoride ions at a temperature of up to 60.degree. C.Type: GrantFiled: November 19, 1986Date of Patent: April 19, 1988Inventor: Bernd Schonfeld
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Patent number: 4720475Abstract: Amorphous, substantially spherical silica particles obtained by acidic hydrolysis of substantially spherical synthetic crystalline calcium silicates having a size of from 20 to 120 microns are coated with a layer comprising silica and alumina. The silica particles obtained may be directly employed as catalysts for the oligomerization of olefins and, having been loaded with platinum, as hydrocracking catalysts.Type: GrantFiled: October 20, 1986Date of Patent: January 19, 1988Assignee: Redco N.V.Inventors: Octavian Anton, Dirk Van Wouwe, Georges Poncelet, Pierre Jacobs, Johan Martens
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Patent number: 4708859Abstract: Precipitation silicas, in the form of aggregates as shown in FIG. 1, having a mean projected area of the aggregates which is higher than about 8,000 nm.sup.2 and preferably is higher than about 15,000 nm.sup.2. The present invention also concerns a process for the production of precipitation silica by maintaining a constant-volume reaction medium to provide a suitable colloids of silica, reacting the colloids with an electrolyte and consolidating the resulting product by the addition of a solution of silicate and an acidifying agent to obtain a precipitation silica.Type: GrantFiled: June 24, 1986Date of Patent: November 24, 1987Assignee: Rhone-Poulenc ChimieInventor: Yvonick Chevallier
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Patent number: 4705771Abstract: Formaldehyde is made from methane and a molecular oxygen containing gas by using a silica supported catalyst having less than 350 parts per million by weight of sodium and having a catalytically effective amount of MoO.sub.3. The low sodium form of the silica support can be made by washing silica gel or precipitated silica, by using a fumed silica or by making an ultrapure form of silica having a silica purity of at least 99.99% silica. The ultrapure form can be made by the hydrolysis of silicon tetraalkoxides. In general, the lower the sodium level, the better is the catalyst.Type: GrantFiled: January 6, 1986Date of Patent: November 10, 1987Assignee: W. R. Grace & Co.Inventor: Nicholas D. Spencer
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Patent number: 4704425Abstract: Improved precipitated silica particulates, well adapted as a pigment or reinforcing filler for curable organosilic polymers and other elastomers, have the properties:______________________________________ (i) BET surface area 190 to 340 m.sup.2 /g (ii) CTAB surface area 180 to 280 m.sup.2 /g (iii) ##STR1## 0.9 to 1.2 (iv) Residual sodium content < 500 ppm (v) pH 3.5 to 6.0 (vi) Specific volume V.sub.o .gtoreq. 4.2 (vii) Amount of particles of a < 0.05%. size as will not pass through a 45.mu.Type: GrantFiled: November 20, 1984Date of Patent: November 3, 1987Assignee: Rhone-Poulenc IndustriesInventors: Robert Lagarde, Jean Machurat, Jean-Claude Morawski, Georges Vrisakis
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Patent number: 4696808Abstract: A process for the preparation of transparent silica gels which can be used as crystal growth media is disclosed. A quantity of cation exchange resin beads is placed in a solution of a soluble potassium salt and stirred for several hours to allow the potassium ions to replace the cations on the resin beads. The supernatant liquid is then decanted through a filter, and the treated resin beads are rinsed with distilled water to remove excess salts. The treated resin beads are then transferred into a sodium silicate solution. The resulting mixture is stirred to allow the potassium ions on the treated resin beads to exchange with the sodium ions in the sodium silicate solution. The treated silicate solution is then poured through a coarse filter. A volume of boiled, cooled distilled water is added to a volume of the treated silicate solution, after which a volume of acetic acid solution is added to the mixture of distilled water and treated silicate solution.Type: GrantFiled: November 24, 1986Date of Patent: September 29, 1987Assignee: The United States of America as represented by the Administrator of the National Aeronautics and Space AdministrationInventors: Patrick G. Barber, Norman R. Simpson
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Patent number: 4690810Abstract: Method for treatment of contaminated chlorosilanes with lime to obtain an environmentally inept silica base product.Type: GrantFiled: March 26, 1986Date of Patent: September 1, 1987Assignee: Union Carbide CorporationInventors: William C. Breneman, David M. Reeser
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Patent number: 4689207Abstract: All silica zeolites are prepared using magadiite as a source of silica.Type: GrantFiled: March 6, 1985Date of Patent: August 25, 1987Assignee: Chevron Research CompanyInventor: Stacey I. Zones
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Patent number: 4683128Abstract: This invention deals with a process for manufacturing high purity silica which comprises making an aqueous alkali silicate solution into fine fibrous gel in a coagulant, treating the fibrous gel obtained with an acid-containing solution, and then with water to extract and remove impurities; and optionallly heating a resulting silica at a temperature of 1,000.degree. C. or higher. Thus obtained silica is preferably used as a filler, especially, the one for resin compositions for encapsulating electronic parts; etc.Type: GrantFiled: June 25, 1986Date of Patent: July 28, 1987Assignees: Nitto Chemical Industry Co., Ltd., Mitsubishi Rayon Co., Ltd.Inventors: Koichi Orii, Masashi Nishida, Junsuke Yagi, Iwao Ohshima
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Patent number: 4681750Abstract: Precipitated amorphous silica useful for manufacturing microporous battery separators is prepared by establishing an aqueous solution of alkali metal silicate having an alkali metal oxide concentration of (a) from 2.1-2.6 grams per liter and a temperature of from about 179.degree. F. to 186.degree. F., or (b) from 5.6 to 7.2 grams per liter and a temperature of from 190.degree. to 198.degree. F.; adding from (a) 14.5 to 19 times or (b) 2 to 5 times respectively the amount of alkali metal silicate initially present in the initial aqueous solution simultaneously with acidifying agent, e.g., sulfuric acid, to the initial aqueous solution while maintaining the initial alkali metal oxide concentration therein substantially constant; reducing the pH of the resulting slurry to from 8 to 9; ageing the slurry at precipitation temperatures for from 15 to 90 minutes; reducing the pH of the aged slurry to from 3.8 to 4.7 and then recovering, e.g.Type: GrantFiled: April 18, 1986Date of Patent: July 21, 1987Assignee: PPG Industries, Inc.Inventors: Harlan B. Johnson, Thomas G. Krivak, David A. Longhini
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Patent number: 4680170Abstract: Crystalline zeolites and zeolitic materials are prepared by crystallization from an aqueous mixture comprising a source of silica, optionally a source of alumina, and an ion-exchange resin preferably an anion-exchange resin. In a preferred form of the invention the anion-exchange resin is in the hydroxide form and the reaction mixture also contains a quaternary ammonium compound.Type: GrantFiled: April 10, 1985Date of Patent: July 14, 1987Assignee: Imperial Chemical Industries PLCInventors: Barrie M. Lowe, Stuart G. Fegan
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Patent number: 4678652Abstract: A process for producing silica in fine powder form, which comprises(a) adding at least one water-miscible alcohol selected from water-miscible monohydric and dihydric alcohols to an aqueous solution of an alkali metal silicate having an SiO.sub.2 concentration of 9 to 20% by weight until a solid precipitate forms and the solution begins, or is about, to become turbid,(b) adding a mineral acid to the resulting mixture in an amount 35 to 80% of the stoichiometrical amount required to neutralize the alkali metal silicate to precipitate silica as a fine powder, and(c) thereafter bringing the resulting slurry into contact with a mineral acid under an acidity of at least 1N.Type: GrantFiled: October 9, 1985Date of Patent: July 7, 1987Assignee: Nippon Sheet Glass Co., Ltd.Inventors: Hiroyuki Tamenori, Akihiko Hattori, Mitsugi Yoshiyagawa
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Patent number: 4666692Abstract: The invention provides a silica-based crystalline material that incorporates titanium into the crystal lattice. A process for preparing this material is also disclosed which is based on the reaction of silica, tetra-alkyl orthotitante and tetrapropyl-ammonium hydroxide.Type: GrantFiled: September 18, 1985Date of Patent: May 19, 1987Assignee: Snamprogetti, S.p.A.Inventors: Marco Taramasso, Giovanni Manara, Vittorio Fattore, Bruno Notari
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Patent number: 4640807Abstract: Silica spheres are prepared in a process comprising:(a) preparing a silica hydrosol by mixing an aqueous solution of an alkali metal silicate with an aqueous solution of an acid;(b) converting the hydrosol into droplet form;(c) aging the droplets in a fluid to produce hydrogel particles;(d) partially drying the hydrogel particles at 10.degree. to 60.degree. C. in air having a relative humidity in the range of from 45 to 95%, to a water content in the range of from 0.3 to 1.3 kg/kg solids;(e) decreasing the cation content of the hydrogel particles by ion-exchange in an aqueous medium to less than 10% w, calculated on dry material; and(f) finally drying the hydrogel particles to obtain silica spheres.Type: GrantFiled: July 24, 1985Date of Patent: February 3, 1987Assignee: Shell Oil CompanyInventors: Madjid Afghan, Josephus G. Sponselee
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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: 4629588Abstract: Adsorbents comprising amorphous silicas with effective average pore diameters of about 60 to about 5000 Angstroms are useful in processes for the removal of trace contaminants, specifically phospholipids and associated metal ions, from glyceride oils.Type: GrantFiled: December 7, 1984Date of Patent: December 16, 1986Assignee: W. R. Grace & Co.Inventors: William A. Welsh, Yves O. Parent
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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: 4613494Abstract: Fluorine in phosphate ores is present as the mineral fluorapatite. When the ores are digested with sulfuric acid a slurry is formed which can be filtered to make wet-process phosphoric acid. But fluorine compounds are discharged into the surrounding air during digestion and filtration. The fluorine-containing air is scrubbed with water to prevent air pollution. Scrubber water is cooled in ponds and is recycled to the scrubber. However, fluorine compounds are emitted from the cooling ponds and cause air pollution. In the present invention, processes are disclosed for treating fluorine-containing gases without use of cooling ponds thereby eliminating the air pollution problem. A facility is provided for treating fluorine-containing gases wherein fluosilicic acid or fluosilicate salts are converted to a fluoride salt by the addition of an alkaline substance. A slightly acidic scrubber water is concentrated in an absorption tower.Type: GrantFiled: January 8, 1985Date of Patent: September 23, 1986Assignee: James C. Barber and Associates, Inc.Inventor: James C. Barber
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Patent number: 4595578Abstract: There is provided an improved process for producing a silica gel having improved pore volume relative to conventional silica gels which comprises the steps of gelling an aqueous alkali metal silicate with an aqueous acid, washing the resulting gel to remove salt or salts and acid, and soaking the gel in an aqueous solution of a water soluble aluminum salt to impart from 0.1% to 0.7% by weight aluminum on the dry basis to said gel, drying and reducing the particle size of the dried gel to from 2.0 to 15 microns, said particles having a pore volume in the range of 1.25 to 2.25 cm.sup.3 /gram. and a product produced by said process.Type: GrantFiled: March 22, 1985Date of Patent: June 17, 1986Assignee: SCM CorporationInventors: Howard J. Cohen, Peter van der Heem, Steven J. Fitch
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Patent number: 4590052Abstract: A precipitated silica having improved morphological characteristics and a process for making precipitated silica. In the precipitated silica of the present invention, the ratio of DBP oil index/CTAB specific surface area is between:7 and 4 for a range of CTAB of between 50-100 m.sup.2 /g,4 and 2.5 for a range of CTAB of between 100-200 m.sup.2 /g,2.5 and 2 for a range of CTAB of between 200-250 m.sup.2 /g,2 and 1.5 for a range of CTAB of between 250-300 m.sup.2 /g, and1.5 and 1.2 for a range of CTAB of between 300-350 m.sup.2 /g.Type: GrantFiled: April 5, 1985Date of Patent: May 20, 1986Assignee: Rhone-Poulenc Chimie de BaseInventors: Yvonick Chevallier, Jean-Claude Morawski
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Patent number: 4582693Abstract: A method is disclosed for making a silica molecular sieve comprising:(A) providing a mixture comprising: water; an oxide, hydroxide or alkoxide of silicon; a mineralizing agent; and a synthesis directing nitrogen containing organic dye; and(B) maintaining said mixture at a temperature of about 80.degree. C. to about 300.degree. C. for an effective period of time to provide said silica molecular sieve.Type: GrantFiled: November 16, 1984Date of Patent: April 15, 1986Assignee: The Standard Oil CompanyInventors: Michael J. Desmond, Frederick A. Pesa, Janie K. Currie
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Patent number: 4581217Abstract: Silica base material for dentifrice having excellent transparency, prolonged stability and desired abrasiveness, has specific surface areas measured by BET method and CTAB method of 5-60 m.sup.2 /g respectively with a difference therebetween of less than 40 m.sup.2 /g, and having a refractive index of 142-1.45. This base material can be prepared by reacting an alkali metal silicate solution with hydrochloric acid or sulfuric acid in the presence of an electrolyte in two stages, a silica crystallization stage in which the pH of the reaction system is brought to 10.0, and a neutralization stage in which the pH of the reaction system is brought to 8.0-6.5, completing the neutralization stage within 30 minutes and aging the neutralized mixture for at least 10 minutes. The ratio of the rate of addition of chloride or sulfate ions between the neutralization and crystallization stages is at least 5:3.Type: GrantFiled: October 17, 1984Date of Patent: April 8, 1986Assignee: Taki Chemical Co., Ltd.Inventors: Shozo Shinpo, Tetsuo Fushino, Akihiro Hachijo, Shozo Ohtsu
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Patent number: 4576921Abstract: The present invention relates to the preparation of materials and finds application in the preparation of dispersions and gels.The invention provides, in one aspect, a process for the preparation of a dispersion which comprises treating a chemical compound with a quaternary ammonium hydroxide so as to peptize the chemical compound to form a dispersion.The dispersion may be, for example, a suspension or a sol (i.e. a colloidal solution). The chemical compound may be, for example, a hydrous metal oxide (e.g. hydrous stannic oxide).Mixed dispersions may be formed in accordance with the present invention.Type: GrantFiled: August 12, 1983Date of Patent: March 18, 1986Assignee: United Kingdom Atomic Energy AuthorityInventor: Edward S. Lane
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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: 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: 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: 4537699Abstract: The present invention provides a process for improving the rheological properties of a suspension of precipitated silica by the addition of an aluminum compound, thereby producing a sprayable suspension or slurry with a pH of greater than 3.5, a solids content of at least about 15% by weight, which may be spray dried to form silica in either powder or microbead form. In a preferred embodiment, the aluminum compound added to the suspension is in the form of sodium aluminate.Type: GrantFiled: November 23, 1983Date of Patent: August 27, 1985Assignee: Rhone-Poulenc Specialites Chimiques "Les Miroirs"Inventor: Jean-Noel Jas
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Patent number: 4508607Abstract: Finely divided particulate silica is prepared by the electrodialysis of sodium silicate solution in the presence of silica-containing nucleation particles (seeds). The novel particulate silica product, herein referred to as dialytic silica, may be used in the preparation of catalysts, sorbents, abrasives, fillers and thickeners.Type: GrantFiled: September 20, 1983Date of Patent: April 2, 1985Assignee: W. R. Grace & Co.Inventor: Milton E. Winyall
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Patent number: RE32503Abstract: A finely divided silicic acid simultaneously suitable as a filtering auxiliary and as a beer stabilizing agent in the filtration of beer. The acid is particulate, and the particles are of an essentially spherical or spheroidal shape with SiO.sub.2 content of at least 95% and an Na.sub.2 O content of less than 0.25%.Type: GrantFiled: November 8, 1984Date of Patent: September 15, 1987Assignee: Akzona IncorporatedInventor: Gerhard Steenken