By Gelling Patents (Class 423/338)
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Patent number: 5616316Abstract: Novel silica particulates especially adapted for formulation to dentifrice compositions exhibit unique physical and chemical properties. In one embodiment, silica particulates have a unique surface chemistry as to be at least 50% compatible with zinc values, and have a number of OH functions, expressed as OH/nm.sup.2, of at most 15 and a zero charge point (PZC) of from 3 to 6.5. In a second embodiment, particulates have a surface chemistry as to be at least 65%, and preferably at least 90% compatible with guanidine values, notably chlorhexidine, and acidity function thereof, Ho, of at least 3.3. In a third embodiment, silica particulates are compatible with organic amines, and have a pH, in aqueous suspension, which varies according to the equations pH.ltoreq.7.5-0.7 log(C) and pH.gtoreq.5.0-0.5 log(C) and which also varies as a function of the electrical conductivity thereof, according to the equations pH.ltoreq.8.5-0.4 log(D) and pH.gtoreq.7.0-0.Type: GrantFiled: June 7, 1995Date of Patent: April 1, 1997Assignee: Rhone-Poulenc ChimieInventor: Jacques Persello
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Patent number: 5614176Abstract: Novel silica particulates especially adapted for formulation to dentifrice compositions exhibit unique physical and chemical properties. In one embodiment, silica particulates have a unique surface chemistry as to be at least 50% compatible with zinc values, and have a number of OH functions, expressed as OH/nm.sup.2, of at most 15 and a zero charge point (PZC) of from 3 to 6.5. In a second embodiment, particulates have a surface chemistry as to be at least 65%, and preferably at least 90% compatible with guanidine values, notably chlorhexidine, and acidity function thereof, Ho, of at least 3.3. In a third embodiment, silica particulates are compatible with organic amines, and have a pH, in aqueous suspension, which varies according to the equations pH.ltoreq.7.5-0.7 log(C) and pH.gtoreq.5.0-0.5 log(C) and which also varies as a function of the electrical conductivity thereof, according to the equations pH.ltoreq.8.5-0.4 log(D) and pH.gtoreq.7.0-0.Type: GrantFiled: June 7, 1995Date of Patent: March 25, 1997Assignee: Rhone-Poulenc ChimieInventor: Jacques Persello
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Patent number: 5614177Abstract: Novel silica particulates especially adapted for formulation to dentifrice compositions exhibit unique physical and chemical properties. In one embodiment, silica particulates have a unique surface chemistry as to be at least 50% compatible with zinc values, and have a number of OH functions, expressed as OH/nm.sup.2, of at most 15 and a zero charge point (PZC) of from 3 to 6.5. In a second embodiment, particulates have a surface chemistry as to be at least 65%, and preferably at least 90% compatible with guanidine values, notably chlorhexidine, and acidity function thereof, Ho, of at least 3.3. In a third embodiment, silica particulates are compatible with organic amines, and have a pH, in aqueous suspension, which varies according to the equations pH.ltoreq.7.5-0.7 log(C) and pH.gtoreq.5.0-0.5 log(C) and which also varies as a function of the electrical conductivity thereof, according to the equations pH.ltoreq.8.5-0.4 log(D) and pH.gtoreq.7.0-0.Type: GrantFiled: June 7, 1995Date of Patent: March 25, 1997Assignee: Rhone-Poulenc ChimieInventor: Jacques Persello
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Patent number: 5612020Abstract: Novel silica particulates especially adapted for formulation to dentifrice compositions exhibit unique physical and chemical properties. In one embodiment, silica particulates have a unique surface chemistry, as to be at least 50% compatible with zinc values, and have a number of OH functions, expressed as OH/nm.sup.2, of at most 15 and a zero charge point (PZC) of from 3 to 6.5. In a second embodiment, particulates have a surface chemistry as to be at least 65%, and preferably at least 90% compatible with guanidine values, notably chlorhexidine, and acidity function thereof, Ho, of at least 3.3. In a third embodiment, silica particulates are compatible with organic amines, and have a pH, in aqueous suspension, which varies according to the equations pH.ltoreq.7.5-0.7 log(C) and pH.gtoreq.5.0-0.5 log(C) and which also varies as a function of the electrical conductivity thereof, according to the equations pH.ltoreq.8.5-0.4 log(D) and pH.gtoreq.7.0-0.Type: GrantFiled: October 26, 1993Date of Patent: March 18, 1997Assignee: Rhone-Poulenc ChimieInventor: Jacques Persello
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Patent number: 5607503Abstract: An insoluble silica based film is formed by placing an ammonium compound and an alcohol as a plasticizing agent in an aqueous solution and blending the aqueous solution with a sodium silicate. The mixture is allowed to condense which produces the insoluble silica-based film. The film is used as a binder, and has particular application as a vehicle in a paint. The invention also describes a method for preparing an insoluble silica-based binder.Type: GrantFiled: September 3, 1993Date of Patent: March 4, 1997Assignee: Refract-A-Gard Pty LimitedInventor: Harley W. Burr
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Patent number: 5589150Abstract: In the present invention, minute spherular silica gel particles suitable as polymer catalyst carriers can easily be obtained without using organic substances simply by controlling the moisture content in a slurry of silica hydrogel particles and water. The obtained spherular silica gel particles have physical properties, such as specific surface area, average pore diameter, and pore volume, that may be easily controlled. The spherular silica gel particles also have sufficient particle strength.Type: GrantFiled: March 4, 1992Date of Patent: December 31, 1996Assignee: Fuji-Davison Chemical Ltd.Inventors: Jiro Kano, Ryuji Orii, Yuzo Horinouchi, Mutsuhiro Ito
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Patent number: 5578101Abstract: The disclosed method of making a glass body by a sol/gel process comprises electrochemically assisted release of the gel body from the mold in which the body was formed. More specifically, the method involves gelation of a sol in a mold that comprises a first conductor member, with a second conductor member also being in contact with the sol and/or gel, and causing the flow of a current between the first and second conductor members, with the first member being the cathode. In consequence of the current flow a substantially liquid lubricating layer that facilitates removal of the gel body from the melt exists at the cathode/gel interface.Type: GrantFiled: September 1, 1995Date of Patent: November 26, 1996Assignee: Lucent Technologies Inc.Inventors: Greg E. Blonder, Robert P. Frankenthal, David W. Johnson, Jr., Eliezer M. Rabinovich
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Patent number: 5576262Abstract: A method of making chromium containing oxide gel-based catalyst wherein an oxide hydrogel is convened to a xerogel by azeotropic distillation of a mixture of said hydrogel and an organic solvent, the improvement comprising impregnating the gel with a chromium compound during azeotropic distillation by incorporating said chromium compound into said mixture before azeotropic distillation and wherein the organic solvent used is selected from the group consisting of ethoxy ethyl acetate, tert-butyoxy propanol, methoxy propyl acetate, n-butoxy propanol, ethoxy ethyl propionate and mixtures thereof.Type: GrantFiled: June 2, 1994Date of Patent: November 19, 1996Assignee: W. R. Grace & Co.-Conn.Inventor: Dean A. Denton
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Patent number: 5573983Abstract: A fine silica tube composed of silica gel and having an outer diameter of 0.05 to 2 .mu.m wherein the cylindrical wall portion of the tube has a cross-section defined by a substantially square outer periphery and a substantially square vacant center, or by a circular outer periphery and a substantially square vacant center; and a fine silica tube composed of silica glass and having an outer diameter of 0.05 to 1.4 .mu.m wherein the cylindrical wall portion of the tube has a cross-section defined by a substantially square outer periphery and a substantially square vacant center. The fine silica gel tube is made by treating a tetraalkoxysilane with ammonia or aqueous ammonia in a water-soluble alcohol medium in the presence of tartaric acid, citric acid, a tartaric acid salt or a citric acid salt, whereby the tetraalkoxysilane is hydrolyzed. The fine silica glass tube is made by calcining the fine silica gel tube at 800.degree. to 1,400.degree. C.Type: GrantFiled: November 7, 1995Date of Patent: November 12, 1996Assignee: Showa Denko Kabushiki KaishaInventors: Hidenori Nakamura, Yasushi Matsui, Takao Goto
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Patent number: 5573674Abstract: A stable activated silica sol is made by reacting sodium aluminum sulfate and a solution of silica. This solution removes suspended particles from aqueous streams rapidly and effectively. The silica sol is stable for many days and thus can be prepared off-site and transported to the point of use. Further, the activated silica or colloidal silica sol solution of the invention can be continuously added to water and waste water streams, or paper making pulps, stocks and furnishes, without danger of solidifying in the transport systems.Type: GrantFiled: October 27, 1995Date of Patent: November 12, 1996Assignee: General Chemical CorporationInventors: Christopher B. Lind, Michael A. Ware
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Patent number: 5571494Abstract: A temperature-activated polysilicic acid is prepared by heating an acidified aqueous alkali metal silicate. The temperature-activated polysilicic acid is used in the production of paper for improvement of retention and water removal.Type: GrantFiled: January 20, 1995Date of Patent: November 5, 1996Assignee: J. M. Huber CorporationInventor: Sakari Saastamoinen
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Patent number: 5565142Abstract: This invention provides an extremely porous xerogel dried at vacuum-to-below supercritical pressures but having the properties of aerogels which are typically dried at supercritical pressures. This is done by reacting the internal pore surface of the wet gel with organic substances in order to change the contact angle of the fluid meniscus in the pores during drying. Shrinkage of the gel (which is normally prevented by use of high autoclave pressures, such that the pore fluid is at temperature and pressure above its critical values) is avoided even at vacuum or ambient pressures.Type: GrantFiled: April 28, 1993Date of Patent: October 15, 1996Inventors: Ravindra Deshpande, Douglas M. Smith, C. Jeffrey Brinker
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Patent number: 5565014Abstract: Sol-gel processing of a silica glass body is facilitated by rapid drying. The body, having been heated to a temperature of about 200.degree. C. in a hermetically sealed vessel, is vented while reducing temperature. Termination of drying coincides with reduction to atmospheric pressure.Type: GrantFiled: March 31, 1994Date of Patent: October 15, 1996Assignee: Lucent Technologies Inc.Inventor: James W. Fleming, Jr.
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Patent number: 5562752Abstract: Heating a wet colloidal gel body in an autoclave above its 1-atmosphere boiling point, under rigorously defined conditions, avoids shrinkage during subsequent drying. As a consequence, drying rates may be increased, and handling care becomes less critical.Type: GrantFiled: March 31, 1994Date of Patent: October 8, 1996Assignee: Lucent Technologies Inc.Inventor: James W. Fleming, Jr.
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Patent number: 5558849Abstract: A process for making inorganic gels by reaction of tetraalkoxy orthosilicates, tetraalkoxy titanates and tetraalkoxy zirconates with strong carboxylic acids. Water need not be present initially as a reactant. Optically clear, very small pore size, narrow pore size distribution, and high specific area inorganic gels useful for abrasion-resistant coatings, optical applications, catalyst or enzyme support, gas separation, or chromatography packing are thus produced.Type: GrantFiled: April 21, 1995Date of Patent: September 24, 1996Assignee: E. I. Du Pont de Nemours and CompanyInventor: Kenneth G. Sharp
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Patent number: 5503820Abstract: An improved method for preparing low-concentration polysilicate microgels from a water soluble silicate and a strong acid in which the silicate and acid are mixed at a rate to produce a Reynolds number of at least 4000, the mixture is aged and then diluted to a silica concentration of not more than 1.0 wt. %. The method achieves reduced silica deposition during the preparation of the microgels.Type: GrantFiled: November 28, 1994Date of Patent: April 2, 1996Assignee: E. I. Du Pont de Nemours and CompanyInventors: Robert H. Moffett, John D. Rushmere
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Patent number: 5500402Abstract: A method for treating a contact body for the exchange of heat or moisture comprises impregnating a contact body with waterglass and treating the impregnated body in acidic and basic environments to form a controlled pore structure.Type: GrantFiled: April 26, 1994Date of Patent: March 19, 1996Assignee: AB Carl MuntersInventor: Hakan Vangbo
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Patent number: 5496527Abstract: A hydrophobic aerogel having excellent transparency is formed by the following process of the present invention. That is, a first gel having a SiO.sub.2 skeleton structure is prepared by hydrolysis and condensation of an alkoxysilane compound in the presence of a solvent. The solvent contained in the first gel is replaced at least partially with a medium to form a second gel. The second gel is reacted with a hydrophobic agent having hydrophobic groups as well as functional groups reactive with silanol groups under a supercritical condition of the medium to form a hydrophobic gel. The medium contained in the hydrophobic aerogel is removed by a supercritical drying method, so that the hydrophobic aerogel having improved transparency and an extremely fine porous structure is obtained.Type: GrantFiled: April 28, 1994Date of Patent: March 5, 1996Assignee: Matsushita Electric Works. Ltd.Inventors: Hiroshi Yokogawa, Masaru Yokoyama, Koichi Takahama, Yuriko Uegaki
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Patent number: 5480582Abstract: A process for synthesizing amorphous silica microspheres having fluorescence behavior includes the steps of placing into a container an organosilicon precursorand with a highly acidic solution and rinsing with a solvate to remove excess of the organosilicon precursor from the amorphous silica microspheres. The organosilicon precursor and the highly acidic solution are immiscible. The process for synthesizing amorphous silica microspheres also includes the steps adding a dopant from a group consisting of rhodamine-6G, rhodamine-B, europium 3.sup.+, fluorescein, coumarin-120, coumarin-314T, thionine, uranium and uranium-sensitized europium, stirring the organosilicon precursor and the highly acidic solution to form droplets of the organosilicon precursor in the highly acidic solution whereby water in the highly acidic solution hydrolizes the droplets of the organosilicon precursor to form amorphous silica microspheres and rinsing with a solvant to remove excess of the organosilicon precursor therefrom.Type: GrantFiled: June 30, 1993Date of Patent: January 2, 1996Inventor: Edward J. A. Pope
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Patent number: 5441718Abstract: A process for making inorganic gels by reaction of tetraalkoxy orthosilicates, tetraalkoxy titanates and tetraalkoxy zirconates with strong carboxylic acids. Water need not be present initially as a reactant. Optically clear, very small pore size, narrow pore size distribution, and high specific area inorganic gels useful for abrasion-resistant coatings, optical applications, catalyst or enzyme support, gas separation, or chromatography packing are thus produced.Type: GrantFiled: September 29, 1993Date of Patent: August 15, 1995Assignee: E. I. Du Pont de Nemours and CompanyInventor: Kenneth G. Sharp
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Patent number: 5425930Abstract: A process for producing microspheres of silica having a maximum diameter of at least 2.5 .mu.m particularly about 2.5 .mu.m to 10 .mu.m from the hydrolysis of a silica precursor, such as a tetraalkoxysilane, which is characterized by employing precursor solutions and feed rates which initially yield a two-phase reaction mixture and beginning the hydrolysis reaction with solutions cooled below ambient temperatures, preferably below about 10.degree. C. Either monodisperse or polydisperse microspheres may be formed.Type: GrantFiled: September 17, 1993Date of Patent: June 20, 1995Assignee: AlliedSignal Inc.Inventor: David J. Anderson
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Patent number: 5419888Abstract: Precipitated silica gels having high surface areas and low oil absorption values are produced by a low temperature synthesis precipitation process. The precipitated silicas have unique flatting characteristics and are additionally useful as conditioning agents for food and salt and in dentifrice formulations.Type: GrantFiled: June 23, 1993Date of Patent: May 30, 1995Assignee: J. M. Huber CorporationInventors: Patrick D. McGill, William C. Fultz
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Patent number: 5409683Abstract: A two-step hydrolysis-condensation method was developed to form metal oxide aerogels of any density, including densities of less than 0.003g/cm.sup.3 and greater than 0.27g/cm.sup.3. High purity metal alkoxide is reacted with water, alcohol solvent, and an additive to form a partially condensed metal intermediate. All solvent and reaction-generated alcohol is removed, and the intermediate is diluted with a nonalcoholic solvent. The intermediate can be stored for future use to make aerogels of any density. The aerogels are formed by reacting the intermediate with water, nonalcoholic solvent, and a catalyst, and extracting the nonalcoholic solvent directly. The resulting monolithic aerogels are hydrophobic and stable under atmospheric conditions, and exhibit good optical transparency, high clarity, and homogeneity. The aerogels have high thermal insulation capacity, high porosity, mechanical strength and stability, and require shorter gelation times than aerogels formed by conventional methods.Type: GrantFiled: July 7, 1994Date of Patent: April 25, 1995Assignee: Regents of the University of CaliforniaInventors: Thomas M. Tillotson, John F. Poco, Lawrence W. Hrubesh, Ian M. Thomas
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Patent number: 5399535Abstract: A reticulated ceramic product is provided having from about 5 to about 95 percent, preferably from about 10 to about 90, percent of the total porosity attributable to mesopores. Reticulated ceramic products provided include silicon oxide, aluminum oxide, zirconium oxide and ruthenium oxide. Reticulated ceramic products are prepared using a porous solid matrix as a template. The reticulated ceramic products are useful as chromatographic media, catalysts and adsorbents.Type: GrantFiled: August 17, 1993Date of Patent: March 21, 1995Assignee: Rohm and Haas CompanyInventor: David W. Whitman
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Patent number: 5395604Abstract: A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2/ g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.Type: GrantFiled: May 3, 1994Date of Patent: March 7, 1995Assignee: Martin Marietta Energy Systems, Inc.Inventors: Michael T. Harris, Osman A. Basaran, Thomas G. Kollie, Fred J. Weaver
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Patent number: 5380510Abstract: This invention provides a method for manufacturing silica gels in a form of scales or needles having a pore volume and a specific surface area being relatively large and being controlled. Silicic acid sol is frozen, crystallized and deposited in gaps among crystal faces of crystals of solvent of the sol, thus obtaining the frozen silica hydrogels in the form of scales or needles. After unfreezing the frozen silica hydrogels, a hydrothermal polymerization is carried out. Subsequently, the silica hydrogels are dried, thus obtaining the silica gels in the form of scales or needles. Furthermore in the invention, by controlling the gelation time period of silica sol, the silica gels with their configuration controlled can result from even inexpensive silica sol. The invention has the advantage that a freeze-drying step is not required: just through freezing, unfreezing, washing and hydrothermal polymerization steps, the physical properties of the silica gels can be controlled.Type: GrantFiled: December 9, 1993Date of Patent: January 10, 1995Assignee: Fuji-Davison Chemical Ltd.Inventors: Takashi Matsui, Nobuki Watanabe, Masayuki Arimura, Eiji Kanemaru, Yuzo Horinouchi, Mutsuhiro Ito
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Patent number: 5376347Abstract: A method of producing uniform inorganic microspheres with a particle size of 0.01 to 500 .mu.m by injecting an aqueous solution containing a particle-forming material into an organic solvent. The method includes injecting the aqueous solution into the organic solvent through a macromolecular membrane having a hydrophobic surface and having pores substantially uniform in pore size and extending in the direction of thickness of the membrane, substantially straight through the membrane, so that a path length of each of the pores corresponds substantially to a thickness of the membrane, to form, in said organic solvent, a large number of emulsion particles substantially uniform in size and then producing uniform inorganic microspheres from said emulsion particles on a one emulsion particle-to-one microsphere basis. The pores in the membrane are formed by either a corpuscular or laser beam.Type: GrantFiled: July 15, 1992Date of Patent: December 27, 1994Assignees: Osaka Gas Company, Limited, Liquid Gas Co., Ltd., Suzuki Yushi Industrial Co., Ltd.Inventors: Masamichi Ipponmatsu, Masashi Nishigaki, Akira Hirano, Tsuyoshi Tsurutani
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Patent number: 5376348Abstract: A method is described for making silica gel having a large active surface area suitable for use as an adsorbent-separator of gases and liquids in hermetically sealed acid accumulators and as a filler in the fabrication of rubber articles.The method produces silica gel having a large active surface area and, at the same time, a microgranular structure. The product is in the form of aggregates having a size which generally does not exceed 5 mm, so no additional grinding of the product is required. The silica gel exhibits a large pore volume.Type: GrantFiled: January 13, 1994Date of Patent: December 27, 1994Assignee: Kamina Ltd.Inventors: Georgi T. Stoilov, Vladimir G. Stoilov, Boiko G. Stoilov, Christo T. Chervenkov, Pavel A. Lazov
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Patent number: 5372796Abstract: A method of making metal oxide clusters in a single stage by reacting a metal oxide with a substoichiometric amount of an acid in the presence of an oxide particle growth terminator and solubilizer. A method of making a ceramer is also disclosed in which the metal oxide clusters are reacted with a functionalized polymer. The resultant metal oxide clusters and ceramers are also disclosed.Type: GrantFiled: April 13, 1993Date of Patent: December 13, 1994Assignee: Southwest Research InstituteInventor: Stephen T. Wellinghoff
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Patent number: 5368833Abstract: Silica sols having a high content of microgel and aluminum modified particles with high specific surface area. The sols can be prepared by a process comprising acidification of a water glass solution, alkalization at a certain dry substance content, particle growth and aluminum modification. The sols are particularly suitable for use as additives, in combination with cationic polymers, in papermaking.Type: GrantFiled: May 8, 1992Date of Patent: November 29, 1994Assignee: Eka Nobel ABInventors: Hans E. Johansson, Bo V. Larsson
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Patent number: 5366645Abstract: A modified amorphous silica is described which, apart from optionally present usual additives, comprises 40 to 85 wt-% silica and 60 to 15 wt-% paraffin, silicone or vegetable oil and/or ethylene glycol. The modified amorphous silica is prepared by bringing together, apart from optionally present usual additives, silica with such a quantity of paraffin, silicone or vegetable oil and/or ethylene glycol that the finished, modified silica has a paraffin, silicone or vegetable oil and/or ethylene glycol content of 60 to 15 wt-%. The modified amorphous silica is suitable as an anti-blocking agent, which can be advantageously prepared as concentrate (masterbatch). Surprisingly, upon preparing such a concentrate the melt-flow index hardly falls compared with the melt-flow index of the polyolefin which forms the basis of the concentrate. Thus it is possible to incorporate large quantities of the modified silica into the concentrate in very homogeneous distribution.Type: GrantFiled: May 15, 1992Date of Patent: November 22, 1994Assignee: W. R. Grace & Co.-Conn.Inventor: Richard Sobottka
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Patent number: 5354548Abstract: This invention provides a three dimensional inorganic oxide structure comprising a myriad of cavities interconnected by holes having a narrow pore size distribution, in which the diameters of the cavities is in the range from 1 to 50 .mu.m and that of the holes in the range 1 to 10 .mu.m and in which the pore volume in the range 1 to 10 .mu.m is at least 2 cc/g and in which the inorganic oxide is selected from alumina, silica, titania, zirconia and mixtures thereof and a process for the preparation of such structures.Type: GrantFiled: November 2, 1992Date of Patent: October 11, 1994Assignee: Unilever Patent Holdings B.V.Inventors: Abraham Araya, Anthony L. Lovell
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Patent number: 5352529Abstract: A thrust vectoring panel which is a hybrid ceramic/ceramic composite consisting of three layers of lightweight materials, the anisotropic properties of which are manipulated such that the properties of the materials, i.e., the coefficient of thermal expansion, the strain energy release rate, and the tensile and flexure modules, either match or gradually transition from material to material. The three layers include a face layer which is of a high temperature capable material that can withstand temperatures within a range of 2300.degree.-25000.degree. F. for an extended period of time and a temperature as high as 28000.degree. F. for a short period of time. The middle layer simply is an insulating layer for providing adequate thermal insulation for the activator mechanism for the thrust panel. The third layer is a skeletal structure or layer which is of a lightweight material having sufficient strength to support all the integral interfaces, such as the activator mounts and the like.Type: GrantFiled: March 3, 1993Date of Patent: October 4, 1994Assignee: Auto-Air Composites, Inc.Inventors: John F. Scanlon, Gary Wigell
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Patent number: 5304364Abstract: A method for preparing inorganic oxide-based materials of spherical form with substantially monomodal distribution, consisting of forming a sol of at least one of the inorganic oxides of interest, adding to said sol a solvent immiscible with the sol, finely dispersing the obtained two-phase mixture into a dispersion of particles of equal diameter, growing said particles by limited coalescence to the desired diameter, gelling said mixture by adding a second solvent containing a gelling agent, and removing the solvent.Type: GrantFiled: October 14, 1992Date of Patent: April 19, 1994Assignee: Istituto Guido Donegani S.p.A.Inventors: Lorenzo Costa, Giulio Boara, Guido Cogliati
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Patent number: 5294480Abstract: A molding based on supercritically dried silica aerogel parts in the form of spherical particles having a diameter of from 0.1 to 10 mm or sheet-like pieces having a thickness of from 2 to 30 mm and a diameter of from 1 to 5 cm, wherein the molding is produced by pressing at from 500.degree. to 1000.degree. C. and at from 0.5 to 10 bar, if necessary under a protective gas, such as nitrogen, without addition of binders.Type: GrantFiled: January 14, 1993Date of Patent: March 15, 1994Assignee: BASF AktiengesellschaftInventors: Manfred Mielke, Guenther Seybold
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Patent number: 5279807Abstract: An improved method and apparatus for preparing low-concentration polysilicate microgels from a water soluble silicate and a strong acid in which the silicate and acid are mixed at a rate to produce a Reynolds number of at least 4000, the mixture is aged and then diluted to a silica concentration of not more than 1.0 wt. %.Type: GrantFiled: May 26, 1992Date of Patent: January 18, 1994Assignee: E. I. du Pont de Nemours and CompanyInventors: Robert H. Moffett, John D. Rushmere
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Patent number: 5275796Abstract: A two-step method is described for making transparent aerogels which have a density of less than 0.003 g/cm.sup.3 to those with a density of more than 0.8 g/cm.sup.3, by a sol/gel process and supercritical extraction. Condensed metal oxide intermediate made with purified reagents can be diluted to produce stable aerogels with a density of less than 0.02 g/cm.sup.3. High temperature, direct supercritical extraction of the liquid phase of the gel produces hydrophobic aerogels which are stable at atmospheric moisture conditions. Monolithic, homogeneous silica aerogels with a density of less than 0.02 to higher than 0.8 g/cm.sup.3, with high thermal insulation capacity, improved mechanical strength and good optical transparency, are described.Type: GrantFiled: September 5, 1991Date of Patent: January 4, 1994Assignee: Regents of the University of CaliforniaInventors: Thomas M. Tillotson, John F. Poco, Lawrence W. Hrubesh, Ian M. Thomas
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Patent number: 5270027Abstract: The invention relates to high-porosity silica xerogels and a process for their preparation consisting of subjecting silica alcogels to thermal treatment in the presence of organic compounds containing amino and hydroxyl groups.The xerogels are characterised by a total pore volume .gtoreq.2 cc/g and a mean pore diameter .gtoreq.100 .ANG..Type: GrantFiled: October 14, 1992Date of Patent: December 14, 1993Assignee: Istututo Guido Donegani S.p.A.Inventors: Luigi Balducci, Franco Montino, Guido Cogliati
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Patent number: 5266533Abstract: SiCxOy where x is greater than zero and up to about 2.0 and y is greater than zero and up to about 2.2 is produced from a cyclosiloxane polymer precursor by pyrolysis in the presence of oxygen by heating at a rate exceeding about 5.degree. C/min.Type: GrantFiled: April 2, 1992Date of Patent: November 30, 1993Assignee: Allied-Signal Inc.Inventors: Roger Y. Leung, John G. Sikonia, Stephen T. Gonczy
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Patent number: 5264197Abstract: An improved sol-gel process for fabricating large, crack-free gel monoliths (e.g., of silica) is described in which a specially-tailored gel microstructure is provided by adjusting the relative concentrations of an alcohol diluent (e.g., ethanol) and/or one or more catalysts (e.g., HCl and HF). Controlled variations in the gel's average pore radius, bulk density, rupture modulus, and elastic modulus over a wide range can be tailored in this fashion. This enables the process to be optimized for the particular application involved.Type: GrantFiled: December 20, 1991Date of Patent: November 23, 1993Assignee: Yazaki CorporationInventors: Shiho Wang, Satyabrata Raychaudhuri, Arnab Sarkar
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Patent number: 5256386Abstract: Silica particles which are substantially spherical, have a particle size of 1 to 100 .mu.m, a very narrow pore size distribution and a low alkali metal content. The particles can be prepared by sol-gel technique using emulsification technique for drop formation. The process comprises a sol growth step in a basic environment based on ammonium or amines and a post-treatment in such an environment. The silica particles are particularly suitable for use in chromatography as they have very good particle and porosity properties and high purity.Type: GrantFiled: June 14, 1990Date of Patent: October 26, 1993Assignee: Eka Nobel ABInventors: Mats Nystrom, Wolgang Herrmann, Bernt Larsson
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Patent number: 5250096Abstract: Relatively large bodies of low-alkali silicate and other glass can be prepared conveniently by a particulate sol-gel process. The glass comprises at least 85 mole % SiO.sub.2, 1-12 mole % oxide of one or more of Li, Na, K, Rb, Cs, Ti and Zr, 0-6 mole % of oxide of Al, and optionally at most 2.5 mole % of oxide of elements other than Si, Li, Na, K, Rb, Cs, Ti, Zr and Al. The process comprises forming particles from a first sol that comprises Si and one or more of Li, Na, K, Rb, Cs, Ti and Zr, and optionally additionally comprises Al. The process further comprises forming a second sol by dispersing the particles in an aqueous liquid, gelling the second sol, and heat treating the resulting gel body such that the glass results.Type: GrantFiled: April 7, 1992Date of Patent: October 5, 1993Assignee: AT&T Bell LaboratoriesInventors: Allan J. Bruce, Eliezer M. Rabinovich
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Patent number: 5242647Abstract: The invention describes a method for making monolithic castings of transparent silica aerogel with densities in the range from 0.001 g/cm.sup.3 to 0.6 g/cm.sup.3. Various shapes of aerogels are cast in flexible polymer molds which facilitate removal and eliminate irregular surfaces. Mold dimensions are preselected to account for shrinkage of alcogel which occurs during the drying step of supercritical extraction of solvent.Type: GrantFiled: July 30, 1991Date of Patent: September 7, 1993Assignee: Regents of The University of CaliforniaInventor: John F. Poco
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Patent number: 5236651Abstract: Particulate ceramic precursor gel compositions (e.g., particulate silica gel) are formed by mechanically extruding a substantially monolithic, substantially undried ceramic precursor. gel through a screen using a mechanical force which is supplied substantially normal to the plane of the screen to directly form the particulate composition, collecting the extrudate in a substantially non-stacked configuration, and drying the extrudate, e.g., in a dryer without imposition of strong vacuum when the extrudate is in substantially nonlayered configuration, to substantially maintain its particle morphology.Type: GrantFiled: December 2, 1991Date of Patent: August 17, 1993Assignee: Akzo N.V.Inventors: Garry J. Garvey, Paul A. Iacobucci, John D. Nowak
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Patent number: 5234673Abstract: Precipitated silica gels having high surface areas and low oil absorption values are produced by a low temperature synthesis precipitation process. The precipitated silicas have unique flatting characteristics and are additionally useful as conditioning agents for food and salt and in dentifrice formulations.Type: GrantFiled: April 24, 1991Date of Patent: August 10, 1993Assignee: J. M. Huber CorporationInventors: Patrick D. McGill, William C. Fultz
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Patent number: 5231059Abstract: A process for preparing an oxidation resistant black glass having the empirical formula SiC.sub.x O.sub.y, wherein 0<x.ltoreq.2.0 and 0<y.ltoreq.2.2. The process comprises reacting cyclosiloxane monomers to effect the bonding of one vinyl carbon atom to a silicon, curing the product at not greater than 250.degree. C., and pyrolyzing at about 800.degree.-1400.degree. C. in an atmosphere containing a sufficient amount of oxygen to reduce the carbon content of the black glass to a desired level.Type: GrantFiled: September 21, 1990Date of Patent: July 27, 1993Assignee: Allied-Signal Inc.Inventors: Roger Y. Leung, Stephen T. Gonczy
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Patent number: 5230953Abstract: Silica particles having an average particle size of 5 to 100 .mu.m, a BET specific surface area of not more than 20 m.sup.2 /g and a pore volume of not more than 0.1 ml/g, each of which has on its surface a plurality of protuberances with a smooth configuration , a diameter at half the protuberance height of the said protuberance being 0.2 to 5.0 .mu.m and a height of the said protuberance being 0.2 to 4.0 .mu.m, and a process for producing the silica particles, which comprises (A) reacting hydrosilicofluoric acid, ammonium silicofluoride or a mixture thereof with ammonia in an aqueous medium to form a silica slurry, (B) separating a silica from the silica slurry, and (C) calcining, after optionally drying, the separated silica at a temperature of not less than 500.degree. C.Type: GrantFiled: December 11, 1990Date of Patent: July 27, 1993Assignee: Nissan Chemical Industries Ltd.Inventors: Makoto Tsugeno, Yasushi Takako, Masao Kubo, Tokumi Mochiyama, Yoshito Yuri
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Patent number: 5229096Abstract: The subject invention is a new type of silica gel and process for producing the same. The silica gel is the product of gelling alkali metal silicate with excess acid in aqueous medium containing a minute amount a polymerization modifier. The modifier and salts from the resulting gel are then leached with water before substantial drying effects have ensued. Spray-dried gel particles do not require the additional steps of aging or ammonia treating to achieve the desired result of high surface area and high pore volume. The gel can be produced to have various useful and unusual characteristics including the combination of high surface area, high pore volume, and a large average pore diameter.Type: GrantFiled: March 12, 1992Date of Patent: July 20, 1993Assignee: SCM Chemicals, Inc.Inventor: Howard J. Cohen
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Patent number: 5227239Abstract: A method is described for making hollow aerogel microspheres of 800-1200 .mu. diameter and 100-300 .mu. wall thickness by forming hollow alcogel microspheres during the sol/gel process in a catalytic atmosphere and capturing them on a foam surface containing catalyst. Supercritical drying of the formed hollow alcogel microspheres yields hollow aerogel microspheres which are suitable for ICF targets.Type: GrantFiled: November 30, 1990Date of Patent: July 13, 1993Assignee: The United States of America as represented by the United States Department of EnergyInventors: Ravindra S. Upadhye, Sten A. Henning
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Patent number: 5215733Abstract: Amorphous silica prepared by the gel route requires washing to remove electrolyte. The gel is formed into small particles by shearing and then washed while being transported by water through stages which separate larger size material. The washing is more rapid than conventional methods and allows the ageing steps to be decoupled from the wash stage.Type: GrantFiled: January 18, 1991Date of Patent: June 1, 1993Assignee: Unilever Patent Holdings B.V.Inventor: John K. Potter